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Home / Applications / Water Analysis for Aldehydes using Post-Column Derivatization by HPLC

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Water Analysis for Aldehydes using Post-Column Derivatization by HPLC

By Miyuki Kanno

PDF IconDownload This Application

January 8, 2024

Introduction

It is a growing concern that aldehydes such as formaldehyde and acetaldehyde may pollute air and water in lakes, reservoirs, and rivers in the environment. Therefore, the aldehydes are subjected to regulations by Air Pollution Control, Water Supply and Offensive Odor Control Acts in Japan.

Pre-column derivatization with 2,4-DNPH is known as a method to measure aldehydes in HPLC, however, the pretreatment of samples such as collection then condensation or extraction is required. JASCO introduced a method for the analysis of formaldehyde and acetaldehyde in water by post-column fluorescence derivatization using 1,3- Cyclohexanedione as derivatization reagent which did not require such pretreatment.

In this report, we extended the applicability of the method to other aldehydes by optimizing the derivatization conditions.

Jasco PU-2080-CO2

Experimental

Keywords

820022H

Results

Figure 1 shows the chemical reaction of 1,3-Cyclohexanedione with aldehydes during the post-column derivatization and figure 2 shows flow path of the system.

Figure 1. Chemical reaction of 1,3-Cyclohexanedione with aldehydes.
Figure 2. Flow line diagram of the system.

No.1 : Eluent
No.2 : Degasser (DG-2080-53)
No.3 : Pump for eluent (PU-2080)
No.4 : Autosampler (AS-2057)
No.5 : Column oven (CO-2060)
No.6 : Column (Shodex RSpak KC-811 6E)
No.7 : Reagent
No.8 : Pump for reagent (PU-2085)
No.9 : Reaction oven (RO-2061)
No.10: Reaction coil
No.11: Cooling coil
No.12: Fluorescence detector (FP-2020)
No.13: Backpressure coil

Figure 3 shows chromatogram of the standard mixture of formaldehyde and acetaldehyde. The two components were separated within 8 minutes.

Figures 4, 5 and 6 show chromatograms of drinking water, river water and rain water, respectively. The top chromatograms are of neat samples and the bottom ones are of samples spiked by adding 0.1 mg/L of formaldehyde and acetaldehyde. All of the samples were separated.

Figure 3. Chromatogram of the standard mixture of formaldehyde and acetaldehyde. 1: Formaldehyde, 2: Acetaldehyde (0.1 mg/L each)
Figure 4. Chromatogram of drinking water.
1: Formaldehyde, 2: Acetaldehyde
Preparation. Drinking water was filtered using 0.45 µm membrane filter.
Figure 5. Chromatogram of river water.
1: Formaldehyde, 2: Acetaldehyde
Preparation. River water was filtered with 0.45 µm membrane filter.
Figure 6. Chromatogram of rain water.
1: Formaldehyde, 2: Acetaldehyde
Preparation: Rain water was filtered with 0.45 µm membrane filter.
This document has been prepared based on information available at the time of publication and is subject to revision without notice. Although the contents are checked with the utmost care, we do not guarantee their accuracy or completeness. JASCO Corporation assumes no responsibility or liability for any loss or damage incurred as a result of the use of any information contained in this document. Copyright and other intellectual property rights in this document remain the property of JASCO Corporation. Please do not attempt to copy, modify, redistribute, or sell etc. in whole or in part without prior written permission.

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About the Author

Miyuki Kanno

JASCO Application Note

Water Analysis for Aldehydes using Post-Column Derivatization by HPLC

Introduction

It is a growing concern that aldehydes such as formaldehyde and acetaldehyde may pollute air and water in lakes, reservoirs, and rivers in the environment. Therefore, the aldehydes are subjected to regulations by Air Pollution Control, Water Supply and Offensive Odor Control Acts in Japan.

Pre-column derivatization with 2,4-DNPH is known as a method to measure aldehydes in HPLC, however, the pretreatment of samples such as collection then condensation or extraction is required. JASCO introduced a method for the analysis of formaldehyde and acetaldehyde in water by post-column fluorescence derivatization using 1,3- Cyclohexanedione as derivatization reagent which did not require such pretreatment.

In this report, we extended the applicability of the method to other aldehydes by optimizing the derivatization conditions.

Jasco PU-2080-CO2

Experimental

Results

Figure 1 shows the chemical reaction of 1,3-Cyclohexanedione with aldehydes during the post-column derivatization and figure 2 shows flow path of the system.

Figure 1. Chemical reaction of 1,3-Cyclohexanedione with aldehydes.
Figure 2. Flow line diagram of the system.

No.1 : Eluent
No.2 : Degasser (DG-2080-53)
No.3 : Pump for eluent (PU-2080)
No.4 : Autosampler (AS-2057)
No.5 : Column oven (CO-2060)
No.6 : Column (Shodex RSpak KC-811 6E)
No.7 : Reagent
No.8 : Pump for reagent (PU-2085)
No.9 : Reaction oven (RO-2061)
No.10: Reaction coil
No.11: Cooling coil
No.12: Fluorescence detector (FP-2020)
No.13: Backpressure coil

Figure 3 shows chromatogram of the standard mixture of formaldehyde and acetaldehyde. The two components were separated within 8 minutes.

Figures 4, 5 and 6 show chromatograms of drinking water, river water and rain water, respectively. The top chromatograms are of neat samples and the bottom ones are of samples spiked by adding 0.1 mg/L of formaldehyde and acetaldehyde. All of the samples were separated.

Figure 3. Chromatogram of the standard mixture of formaldehyde and acetaldehyde. 1: Formaldehyde, 2: Acetaldehyde (0.1 mg/L each)
Figure 4. Chromatogram of drinking water.
1: Formaldehyde, 2: Acetaldehyde
Preparation. Drinking water was filtered using 0.45 µm membrane filter.
Figure 5. Chromatogram of river water.
1: Formaldehyde, 2: Acetaldehyde
Preparation. River water was filtered with 0.45 µm membrane filter.
Figure 6. Chromatogram of rain water.
1: Formaldehyde, 2: Acetaldehyde
Preparation: Rain water was filtered with 0.45 µm membrane filter.

Keywords

820022H

This document has been prepared based on information available at the time of publication and is subject to revision without notice. Although the contents are checked with the utmost care, we do not guarantee their accuracy or completeness. JASCO Corporation assumes no responsibility or liability for any loss or damage incurred as a result of the use of any information contained in this document. Copyright and other intellectual property rights in this document remain the property of JASCO Corporation. Please do not attempt to copy, modify, redistribute, or sell etc. in whole or in part without prior written permission.
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