Analysis of Phenols in Water

Chromatography Forum: GC Archives: Analysis of Phenols in Water
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Sean Sweeney on Friday, July 7, 2000 - 06:37 am:

I need to develop a mehtod for the analysis of Phenol and/or Bromophenol in water. I need to reach levels of 10 mg/l . I have a PE Autosystem XL with Programable Pressure and Temprature Split Splitless Injectors. A SGE BP1 column and can use either a TCD or FID. This procedure would replace a chloroform extraction/Colourometric method so I would greatly appreciate any assistance that can be offered.
Thanks Sean


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Friday, July 7, 2000 - 08:15 am:

My bet is that if you used HPLC you could determine these phenols' levels directly, without extraction. My company has assayed for trace levels of phenolic compounds in rinse water easily using RP-18 columns, acetic acid-water-ACN mobile phase, and UV at 280 nm with no extraction or clean up.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Sean Sweeney on Friday, July 7, 2000 - 08:23 am:

Thanks Anon
But unfortunatly I don't have access to HPLC and require a GC solution to this problem. Any other comments would be greatly appreciated. I would also like to hear form anyone using Thermal Desorption for Occupational Exposure monitoring with a particular interest in Adsorbents for use with C2-C5 alcohols.
Thanks again Sean


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Russ on Monday, July 10, 2000 - 06:25 am:

There are several GC methods for phenols in supplier catalogs. Some to check:
Supelco http://www.sigma-aldrich.com
Restek http://www.restekcorp.com
SGE http://www.sge.com
J&W http://www.jandw.com
Most GC column or suppliers probably have applications you might be able to adapt.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Sean Sweeney on Monday, July 10, 2000 - 08:37 am:

Thanks for the advice Russ
Sean


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Bill Jenko on Sunday, July 16, 2000 - 08:55 pm:

At the 10 ppm level, you can probably do this by direct injection if you have an on-column or other direct injection insert for a 0.53mm ID capillary column. You will need the FID. Acidify your sample with a strong acid (sulfuric works) and shoot. I presume this is a wastewater or some other sample with high dissolved solids, so if you inject on-column you will deposit a fair amount of trash on the column and have to cut a few inches of the column off every so often. There are nice inserts for packed column injectors to adapt them to 0.53 mm ID capillaries, and these inserts can be packed with glass wool or something to collect the nonvolatile trash in your sample.

I don't recommend a splitless injection with water as the solvent, particularly with BP-1.

If you don't mind extractions, acidify your sample, extract in Isopropyl Ether (use about 10mL of IPE for every 100 mL of sample), inject about 1 uL splitless (set the split vent to open at about 30-60 seconds or thereabouts) into your BP-1 column and it should look very nice. Watch for the Hydroquinone peak in your Isopropyl Ether. Hydroquinone is used as a preservative in IPE. The Phenol, the Xylenols and Cresols all elute before Hydroquinone, if I remember correctly (it was about 15 years ago). I don't know where Bromophenol comes out.

Good Luck!


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Sean Sweeney on Monday, July 17, 2000 - 03:43 am:

Thanks a million Bill I will try out your suggestions.
Sean


Top of pagePrevious messageNext messageBottom of pageLink to this message  By ajtony on Wednesday, February 28, 2001 - 03:28 am:

One year ago we analysed the phenol in water with SPME (Solid Phase Micro Extraction, Supelco followed GC/MS determination.
SPME conditions were:
SPME fiber: 85 um polyacrylate fiber with immersion.
Extraction time: 20 min. with high speed stirring
Extraction volume: 4 ml. Water was saturated with NaCl
Desorption temp: 280 oC
Desorptiom time: 5 min
Limit of detection: less than 1 ug/L

Zsolt Ajtony


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