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Method for determination of organic hydroperoxides

A hydroperoxide, organic technology, applied in the field of analysis for the determination of organic pollutants in wastewater streams, can solve the problem of not proposing to measure the concentration of organic hydroperoxides, etc.

Inactive Publication Date: 2007-10-31
SUNOCO INC (R&M)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, none of these references propose measuring the concentration of organic hydroperoxides in aqueous solutions

Method used

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  • Method for determination of organic hydroperoxides
  • Method for determination of organic hydroperoxides
  • Method for determination of organic hydroperoxides

Examples

Experimental program
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Embodiment 1

[0023] A common organic hydroperoxide in the wastewater effluent stream of a phenol plant is cumene hydroperoxide (CHP), which is the precursor of phenol in this process. When treated with acetic acid and potassium iodide, cumene hydroperoxide decomposes to dimethylphenylcarbinol (DMPC, also known as dimethylbenzyl alcohol or DMBA). The method of the present invention for measuring CHP in wastewater streams is performed using the following procedure.

[0024] A series of samples of DMPC in water were prepared at different dilutions to determine the percent recovery of DMPC from aqueous solutions by headspace gas chromatography. Samples were prepared in deionized water and in water with low and high concentrations of salt. The salt solution was used to simulate the qualities of wastewater streams typically found in phenol plants. Samples were prepared with and without the reagents used to derivatize CHP, namely acetic acid and potassium iodide. Table 1 shows these experiment...

Embodiment 2

[0040]Various process streams were analyzed for cumene hydroperoxide (CHP) and methyl hydroperoxide using the method of the present invention. All samples containing significant amounts of salt were diluted 1:10 with water prior to preparation and analysis. CHP is detected as DMPC and MHP is detected as methanol (MeOH). Tables 5 to 10 show the results of the analysis of various process streams from the phenol plant. Native methanol and DMPC were determined from underivatized "as is" samples. A second set of samples was derivatized according to the invention by adding a 1 mL aliquot of a diluted water stream, 0.10 mL of acetic acid, 0.15 mL of 50% aqueous potassium iodide and 0.75 mL of water. Actual MHP and CHP concentrations were calculated from the difference in methanol and DMPC concentrations (corrected for dilution and percent recovery) between the "as is" and derivatized samples.

[0041] Element

[0042] Element

[0043] Element

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Abstract

The concentration of an organic hydroperoxide in an aqueous stream is determined by derivatizing the organic hydroperoxide to the corresponding alcohol by addition of acetic acid and potassium iodide. The corresponding alcohol is then quantified by headspace gas chromatography and correlated to a concentration of the organic hydroperoxide in the aqueous stream.

Description

technical field [0001] The present invention generally relates to the field of analytical methods for the determination of organic pollutants in wastewater streams. More specifically, the present invention relates to gas chromatography methods for the determination of organic contaminants in aqueous streams. Background of the invention [0002] In industrial processes, an ongoing environmental focus is the organic content of wastewater streams. Of particular concern in a variety of processes are organic hydroperoxides, either used as catalysts or reactants in the process, or produced as by-products of the process. [0003] Various methods for the detection of hydroperoxides as well as organic hydroperoxides in solution are described in the literature. For example, iodometry involves reacting hydroperoxide with iodide ions (such as potassium iodide or sodium iodide) and acetic acid to produce iodine, which can then be measured colorimetrically by titration. Another titrati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N1/22G01N33/18
CPCG01N2001/2229G01N33/1826G01N30/06C04B2237/366Y10T436/206664C01B15/00G01N1/22G01N33/18G01N33/00
Inventor R·B·克里彭R·W·恩布利奇
Owner SUNOCO INC (R&M)