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Section: 8 | Instability of HPLC Solvents |
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The recommended form of citation is:
John R. Rumble, ed., CRC Handbook of Chemistry and Physics, 103rd Edition (Internet Version 2022), CRC Press/Taylor & Francis, Boca Raton, FL.
If a specific table is cited, use the format: "Physical Constants of Organic Compounds," in CRC Handbook of Chemistry and Physics, 103rd Edition (Internet Version 2022), John R. Rumble, ed., CRC Press/Taylor & Francis, Boca Raton, FL.

INSTABILITY OF HPLC SOLVENTS

Thomas J. Bruno and Paris D. N. Svoronos

Solvents that are commonly used in high-performance liquid chromatography frequently have inherent chemical instabilities that must be considered when designing an analysis or in the interpretation of results (Refs. 1-4). In many cases, such solvents are obtainable with stabilizers added to control the instability or to slow the reaction. Reactive solvents that do not have stabilizers must be used quickly or be given proper treatment. In either case, it is important to understand that the solvents (as they may be used in an analysis) are not necessarily pure materials.

Although not specifically considered below, the preparation of aqueous-organic solvents for HPLC can cause the introduction of impurities. Mixing acetonitrile and water is endothermic and can sometimes exacerbate air dissolution. Buffers are also a special case in that the pH can change due to exposure to air and the development of microbes (Ref. 4). Buffers should be used the same day of preparation and often incorporate the preservative sodium metabisulfite.

Column definitions for the table are as follows.

Column heading Definition
Name Solvent name
Mol. form. Molecular formula of solvent
Contaminants, reaction products Typical contaminants and reaction products found in the solvent
Stabilizers Common stabilizers used with the solvent

References

  1. Sadek, P. C., The HPLC Solvent Guide, Second Edition, Wiley Interscience, New York, 2002.
  2. Bruno, T. J., and Straty, G. C., J. Res. Natl. Bur. Stds. (U.S.), 91, 135, 1986. [https://doi.org/10.6028/jres.091.021]
  3. Straty, G. C., Palavra, A. M. F., and Bruno, T. J., Int. J. Thermophys. 7, 1077, 1986. [https://doi.org/10.1007/BF00502379]
  4. Bruno, T. J., and Svoronos, P. D. N., CRC Handbook of Basic Tables for Chemical Analysis – Data-Driven Methods and Interpretation, Fourth Edition, CRC Press/Taylor & Francis, Boca Raton, FL, 2021. [https://doi.org/10.1201/b22281]
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Characteristics of HPLC Solvents



NameMol. form.Contaminants, reaction productsStabilizers
Ethers
Diethyl ether(C2H5)2OPeroxides12–3% (vol/vol) ethanol2
1–10 ppm (mass/mass) BHT3
(1.5–3.5% ethanol) + (0.2–0.5% water) + (5–10 ppm (mass/mass) BHT3)
Diisopropyl etherC6H14OPeroxides10.01% (mass/mass) hydroquinone
5–100 ppm (mass/mass) BHT3
1,4-DioxaneC4H8O2Peroxides125–1500 ppm (mass/mass) BHT3
TetrahydrofuranC4H8OPeroxides125–250 ppm (mass/mass) BHT3
Chlorinated Alkanes
TrichloromethaneCHCl3Hydrochloric acid, chlorine, phosgene (CCl2O)0.5–1% (vol/vol) ethanol
50–150 ppm (mass/mass) amylene4
various ethanol amylene blends
DichloromethaneCH2Cl2Hydrochloric acid, chlorine, phosgene (CCl2O)25 ppm (mass/mass) amylene
25 ppm (mass/mass) cyclohexene
400–600 ppm (mass/mass) methanol
various amylene methanol blends
Alcohols
EthanolC2H5OHWater, numerous denaturants are commonly added
MethanolCH3OHWater; formal dehydrate (at elevated temperature)
Ketones
Acetone(CH3)2CODiacetone alcohol, and higher oligomers

  • 1The peroxide concentration that is usually considered hazardous is 250 ppm (mass/mass).
  • 2Ethanol does not actually stabilize diethyl ether, nor is it a peroxide scavenger, although it was thought to be so in the past. It is still available in chromatographic solvents to preserve the utility of retention relationships and analytical methods.
  • 32,6-Di-tert-butyl-p-cresol.
  • 4Amylene is a generic name for 2-methyl-2-butene.


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