Anionic Surfactant (LAS) Analysis


Chemical Name: Sodium Dodecylbenzene Sulfonate
Molecular Formula: C16H25NaO3S

Anionic surfactants which are contaminated from factory wastewater and domestic sewage are considered to be an important indicator of water pollution because they cause foaming when present in water. Linear alkylbenzene sulfonic acid (LAS), a kind of anionic surfactant, is used in the largest amount among synthetic detergents. For anionic surfactants, standard values are set for Drinking Water Quality Standards and Environmental Quality Standards for Water Pollution in Japan.
Fujifilm Wako provides various standard solutions for anionic surfactants that are subject to measurement in Japanese Drinking Water Quality Standards, internal standard solutions that can be used for LC/MS, and HPLC columns.

Standard Solution

Five types of anionic surfactants that are subject to measurement in Japanese Drinking Water Quality Standards (sodium decylbenzenesulfonate, sodium undecylbenzenesulfonate, sodium dodecylbenzenesulfonate, sodium tridecylbenzenesulfonate, and sodium tetradecylbenzenesulfonate, their phenyl group is bonded to a carbon other than the terminal of a linear-chain alkyl group). You can use them for calibration curve creation.
In addition, Fujifilm Wako also offers a mixture standard solution in which the above five anionic surfactants are mixed at 1 mg/mL each (methanol solution).

Mixture standard solution

LAS (C10-C14), in which a phenyl group is bonded to carbons other than the terminal of the linear alkyl chain, are mixed. And the concentration values of each LAS are specified. It can be used for the notification test method of the Japanese Drinking Water Quality Standards.

Code No. Product Name Grade Volume
013-20131 Anionic Surfactants Mixture Standard Solution (each 1 mg/mL Methanol Solution) for Water Analysis 1 mL x 5 A
  • [HPLC Chromatogram]00343_img02.png
  • [Composition information]
    Peak No. Anionic Surfactant
    C10 Sodium Decylbenzenesulfonate
    C11 Sodium Undecylbenzenesulfonate
    C12 Sodium Dodecylbenzenesulfonate
    C13 Sodium Tridecylbenzenesulfonate
    C14 Sodium Tetradecylbenzenesulfonate
  • [HPLC conditions]
    Column Wakopak® Navi C18-5 4.6 mm x 250 mm
    Column temperature 40℃
    Eluent 0.1 mol/L NaClO4 in CH3CN/H2O= 65/35
    Flow rate 1.0 mL/min.
    Detection UV 225 nm

Single Standard Solution

Code No. Product Name Grade Volume
195-13111 Sodium Decylbenzenesulfonate Standard Solution (1 mg/mL Methanol Solution) for Water Analysis 1 mLx5 A
192-13121 Sodium Undecylbenzenesulfonate Standard Solution (1 mg/mL Methanol Solution) for Water Analysis 1 mLx5 A
199-13131 Sodium Dodecylbenzenesulfonate Standard Solution (1 mg/mL Methanol Solution) for Water Analysis 1 mLx5 A
196-13141 Sodium Tridecylbenzenesulfonate Standard Solution (1 mg/mL Methanol Solution) for Water Analysis 1 mLx5 A
193-13151 Sodium Tetradecylbenzenesulfonate Standard Solution (1 mg/mL Methanol Solution) for Water Analysis 1 mLx5 A

Internal Standard Solution

Fujifilm Wako provides internal standard solutions that can be used for LC/MS analysis of anionic surfactants. Sodium 4-Dodecylbenzenesulfonate-13C6 Standard Solution has physical properties close to those of C12-LAS, which is subject to various regulations in Japan, and can be used as an internal standard.

Internal standard solution

Code No. Product Name Grade Volume
195-17131 Sodium p-n-Octylbenzenesulfonate Standard Solution (1 mg/mL Methanol Solution) for Water Analysis 1 mL
191-19171 Sodium 4-Dodecylbenzenesulfonate-13C6 Standard Solution (10 μg/mL Methanol Solution) for Water Analysis 1 mL x 5 A

Solid Phase Extraction Column

Recovery test of sodium alkylbenzenesulfonate (C10-C14) in water samples using Presep®-C C18 and Presep®-Agri

(Compliant with the Japanese Drinking Water Quality Standards (enforced on April 1, 2004))

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HPLC Column

Wakopak® Wakosil-Ⅱ

LC/MS/MS analysis example of LAS (C10-C14) using the Japanese Drinking Water Quality Standards notification method (HPLC column: Wakopak® Wakosil-Ⅱ 3C8RS)

LC/MS/MS Chromatogram
00343_img15.png
LAS Monitoring Ions (m/z) Mode LAS Monitoring Ions (m/z) Mode LAS Monitoring Ions (m/z) Mode
Precursor Products Precursor Products Precursor Products
C10-LAS 297 183 - C12-LAS 325 183 - C14-LAS 353 183 -
C11-LAS 311 183 - C13-LAS 339 183 - 13C12-LAS 331 176 -
Analysis conditions
[Instrument]

Shimadzu LC/MS-8040

[HPLC]
Column: Wakopak® Wakosil-Ⅱ 3C18RS 2.0×150 mm
Column temperature: 40℃
Eluent: A) H2O, B) CH3CN
Gradient:
Time (min.) B conc. (%)
0-30 60
Flow rate: 0.3 mL/min.
[MS]

Ionization: ESI
Mode: MRM

LC/MS/MS analysis example of LAS (C10-C14) using the Japanese Drinking Water Quality Standards notification method (HPLC column: Wakopak® Wakosil-Ⅱ 3C18HG)

LC/MS/MS Chromatogram
00343_img05.png
LAS Monitoring Ions (m/z) Mode LAS Monitoring Ions (m/z) Mode LAS Monitoring Ions (m/z) Mode
Precursor Products Precursor Products Precursor Products
C10-LAS 297 183 - C12-LAS 325 183 - C14-LAS 353 183 -
C11-LAS 311 183 - C13-LAS 339 183 - 13C12-LAS 331 176 -
Analysis conditions
[Instrument]

Shimadzu LC/MS-8040

[HPLC]
Column: Wakopak® Wakosil-Ⅱ 3C18HG 2.0×150 mm
Column temperature: 40℃
Eluent: A) 0.1 vol% HCOOH in H2O, B) 0.1 vol% HCOOH in CH3CN
Gradient:
Time (min.) B conc. (%)
0-30 75
Flow rate: 0.3 mL/min.
[MS]

Ionization: ESI
Mode: MRM

Wakopak® Wakosil® AS-Aqua

Linear alkylbenzene sulfonic acid (LAS) exists as a mixture of isomers, and many peaks are detected when use ODS columns.
Wakopak® Wakosil® AS-Aqua separates isomers as a single peak for each carbon length of LAS, which improves detection sensitivity, simplifies quantitative calculations, and shortens analysis time. Also, since the linear alkylbenzene sulfonic acids (LAS) and branched alkylbenzene sulfonic acids are separated, they can be distinguished. Furthermore, there is no significant difference in the measured values compared to a general ODS column, and more accurate measurements can be performed even in the low-concentration condition.

Comparison of ODS Columns and Wakopak® Wakosil® AS-Aqua for Anionic Surfactant Analysis

[HPLC]

Eluent CH3CN/H2O=65/35 (v/v)+ 12.3 g/1,000 mL NaClO4 added
Flow rate 1.0 mL/min. (Wakopak® Navi C18-5), 0.7 min. (Wakopak® Wakosil® AS-Aqua)
Detection FL Ex. 221 nm, Em. 284 nm
Injection volume 10 µL
Sample Anionic Surfactants Mixture Standard Solution (C10-C14 each 10 mg/mL Methanol Solution)

Column: Wakopak® Navi C18-5 4.6 mmx250 mm (ODS column)

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Column: Wakopak® Wakosil® AS-Aqua*

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* Wakopak® Wakosil® AS-Aqua can recognize and separate both linear and branched alkylbenzene sulfonic acids.

Separation of anionic surfactants mixture standard solution and toluene

Depending on the pretreatment method, toluene may be mixed in the extracted sample.

When using Wakopak® Wakosil® AS-Aqua, toluene and anionic surfactants are eluted separately, allowing analysis without interference from the toluene peak.

  • 00343_img12.png
  • [HPLC]
    Column : Wakopak® Wakosil® AS-Aqua 4.6 mm x 250 mm
    Column temperature : 40℃
    Eluent : CH3CN/H2O = 65/35 (v/v) + 12.3 g/1,000 mL NaClO4 added
    Flow rate : 0.7 mL/min.
    Detection : (Upper) FL Ex. 221 nm. Em. 284 nm (Lower) UV 225 nm
    Injection volume : 10 μL
    Sample : Anionic Surfactants Mixture Standard Solution
     (C10-C14 each 10 mg/mL Methanol Solution)+Toluene (1 μL/mL) added

Product List

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Mixture Standard Solution

Single Standard Solution

Internal Standard Solution

HPLC Column

Dedicated Eluent for Wakopak Wakosil AS-Aqua

Solid Phase Extraction Column

Related Product List

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Author: E. Leung

For research use or further manufacturing use only. Not for use in diagnostic procedures.

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