Silica Gel for Dioxin and PCBs Analysis
Dioxins and PCBs are analyzed in various fields such as soil, sediment, surface water, exhaust gas samples from garbage incinerationfacilities, food samples including olive oil etc. Pre-treatment by sulfuric acid is used as a clean-up method for contaminants such aspigments, lipids and polycyclic aromatic hydrocarbons (PAHs) contained in samples. However, standard operation is very complicatedand time consuming. In order to simplify these procedures, silica gel impregnated with 55% sulfuric acid is helpful. Increasing the sulfuric acid content from ordinary 22% or 44% to 55% maximize the removal capacity and shows almost the sameperformance as batch or column treatments. Furhermore, this material is applicable to POPs pesticide and waste oil analsis, in additionto dioxin analysis.
FUJIFILM Wako provides unmodified silica gel (Wakogel® DX, Wakogel® S-1), and chemically modified silica gel which is modified by sulfuric acid, silver nitrate, and potassium hydroxide, that can be used for dioxin / PCB analysis.
Wakogel® DX
This silica gel guarantees for a low concentration of dioxins.
Dioxins
-
PCDDs
Requirement Specification 2,3,7,8-Tetra-CDD Less than 5 pg/10 g 1,3,6,8-Tetra-CDD Less than 5 pg/10 g 1,3,7,9-Tetra-CDD Less than 5 pg/10 g 1,2,3,7,8-Penta-CDD Less than 5 pg/10 g 1,2,3,4,7,8-Hexa-CDD Less than 5 pg/10 g 1,2,3,6,7,8-Hexa-CDD Less than 5 pg/10 g 1,2,3,7,8,9-Hexa-CDD Less than 5 pg/10 g 1,2,3,4,6,7,8-Hepta-CDD Less than 5 pg/10 g Octa-CDD Less than 10 pg/10 g -
PCDFs
Requirement Specification 2,3,7,8-Tetra-CDF Less than 5 pg/10 g 1,3,6,8-Tetra-CDF Less than 5 pg/10 g 1,2,3,7,8-Penta-CDF Less than 5 pg/10 g 2,3,4,7,8-Penta-CDF Less than 5 pg/10 g 1,2,3,4,7,8-Hexa-CDF Less than 5 pg/10 g 1,2,3,6,7,8-Hexa-CDF Less than 5 pg/10 g 1,2,3,7,8,9-Hexa-CDF Less than 5 pg/10 g 2,3,4,6,7,8-Hexa-CDF Less than 5 pg/10 g 1,2,3,4,6,7,8-Hepta-CDF Less than 5 pg/10 g 1,2,3,4,7,8,9-Hepta-CDF Less than 5 pg/10 g Octa-CDF Less than 10 pg/10 g
Co-PCBs
-
Non-ortho PCBs
Requirement Specification 3,4,4',5-Tetra-CB Less than 10 pg/10 g 3,3',4,4'-Tetra-CB Less than 10 pg/10 g 3,3',4,4',5-Penta-CB Less than 10 pg/10 g 3,3',4,4',5,5'-Hexa-CB Less than 10 pg/10 g -
Mono-ortho PCBs
Requirement Specification 2',3,4,4',5-Penta-CB Less than 10 pg/10 g 2,3',4,4',5-Penta-CB Less than 10 pg/10 g 2,3,4,4',5-Penta-CB Less than 10 pg/10 g 2,3,3',4,4'-Penta-CB Less than 10 pg/10 g 2,3',4,4',5,5'-Hexa-CB Less than 10 pg/10 g 2,3,3',4,4',5-Hexa-CB Less than 10 pg/10 g 2,3,3',4,4',5'-Hexa-CB Less than 10 pg/10 g 2,3,3',4,4',5,5'-Hepta-CB Less than 10 pg/10 g
Wakogel® S-1
Silica gel specialized for the separation and purification of PCBs and organochlorine pesticides, with guaranteed PCB resolution by test "Suitability for PCB determination".
Suitability for PCB determination
Operation
Judgment
① Resolution: More than 60%
C: Resolution (%)
ni: First fraction that eluted p,p'-DDE
D: The total of peak heights of PCBs eluted in all fractions less than ni
E: The total of peak heights of PCBs eluted after the 25th fractions
(Subtract the p, p'-DDE peak from the sum of all detected peaks)
② Elution:
26th fractions …Detect p,p'-DDE, p,p’-DDT, and γ-BHC.
27th fractions …Almost no p,p’-DDE, p,p‘-DDT and γ-BHC detected.
Procedure (55% Sulfuric Acid-impregnated Silica Gel)
- Take 10ml of extracted crude hexane solution for 90g of soil.
- Add 3g of 55% sulfuric acid silica gel.
- Stir well for 30 sec.
- Filter the supernatant solution.
Data (55% Sulfuric Acid-impregnated Silica Gel)
Blank data for 55% sulfuric acid silica gel
| PCDDs/Fs | Actual Value (fg/g) |
DL-PCBs(Dioxin Like-PCBs) | Actual Value (fg/g) |
|---|---|---|---|
| 2,3,7,8-TeCDD | 25 max. | 3,4,4',5-TeCB（#81） | 30 max. |
| 1,2,3,7,8-PeCDD | 25 max. | 3,3',4,4'-TeCB（#77） | 30 max. |
| 1,2,3,4,7,8-HｘCDD | 30 max. | 2,3',4,4',5-PeCB（#118） | 30 max. |
| 1,2,3,6,7,8-HｘCDD | 30 max. | 2,3,4,4',5-PeCB(#114) | 30 max. |
| 1,2,3,7,8,9-HｘCDD | 30 max. | 2,3,3',4,4'-PeCB（#105） | 30 max. |
| 1,2,3,4,6,7,8-HｐCDD | 30 max. | 3,3',4,4',5-PeCB（#126） | 30 max. |
| 1,2,3,4,6,7,8,9-OCDD | 50 max. | 2',3,4,4',5-PeCB(#123) | 30 max. |
| 2,3,7,8-TeCDF | 25 max. | 2,3',4,4',5,5'-HｘCB(#167) | 30 max. |
| 1,2,3,7,8-PeCDF | 25 max. | 2,3,3',4,4',5-HｘCB（#156） | 30 max. |
| 2,3,4,7,8-PeCDF | 25 max. | 2,3,3',4,4',5'-HｘCB（#157） | 30 max. |
| 1,2,3,4,7,8-HｘCDF | 30 max. | 3,3',4,4',5,5'-HｘCB（#169） | 30 max. |
| 1,2,3,6,7,8-HｘCDF | 30 max. | 2,3,3',4,4',5,5'-HpCB(#189) | 30 max. |
| 1,2,3,7,8,9-HｘCDF | 30 max. | ||
| 2,3,4,6,7,8-HｘCDF | 30 max. | ||
| 1,2,3,4,6,7,8-HｐCDF | 30 max. | ||
| 1,2,3,4,7,8,9-HｐCDF | 30 max. | ||
| 1,2,3,4,6,7,8,9-OCDF | 50 max. |
Application (55% Sulfuric Acid-impregnated Silica Gel)
Ability to remove PAHs by 55% sulfuric acid silica gel
Clean-up effect by combining with multi-layer silica gel column
References
- JP5691120 B2 (2015)
- Ito, T. et al.: Proceedings of the 17th Symposium of Environmental Chemistry (2008)
- Ito, T. et al.: Proceedings of the 9th Symposium of Environmental Chemistry (2000)
- Ito, T. et al.: Proceedings of the 14th Symposium of Environmental Chemistry (2005)
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Silica gel
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