GB2576949A - Method for measuring optical brighteners in environmental water - Google Patents

Method for measuring optical brighteners in environmental water Download PDF

Info

Publication number
GB2576949A
GB2576949A GB1814675.3A GB201814675A GB2576949A GB 2576949 A GB2576949 A GB 2576949A GB 201814675 A GB201814675 A GB 201814675A GB 2576949 A GB2576949 A GB 2576949A
Authority
GB
United Kingdom
Prior art keywords
water
organic solvent
optical brighteners
volume
environmental
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
GB1814675.3A
Other versions
GB201814675D0 (en
Inventor
Nicholas Mayers Carl
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
UK Secretary of State for Defence
Original Assignee
UK Secretary of State for Defence
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by UK Secretary of State for Defence filed Critical UK Secretary of State for Defence
Priority to GB1814675.3A priority Critical patent/GB2576949A/en
Publication of GB201814675D0 publication Critical patent/GB201814675D0/en
Publication of GB2576949A publication Critical patent/GB2576949A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18Water
    • G01N33/1826Organic contamination in water
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • G01N21/88Investigating the presence of flaws or contamination
    • G01N21/94Investigating contamination, e.g. dust
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18Water
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • G01N2001/4061Solvent extraction
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7769Measurement method of reaction-produced change in sensor
    • G01N2021/7786Fluorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

A method for measuring the concentration of optical brighteners in an environmental water source comprising: collecting a sample of water from an environmental source; adding to the sample an organic solvent that is immiscible with water, where the volume of the organic solvent is 5% or less of the volume of the water sample; adding to the water and organic solvent mixture cetyl trimethylammonium bromide as a detergent/phase-transfer agent and agitating the resultant mixture; allowing the water and organic solvent to re-separate following agitation and then removing the organic solvent from the mixture; adding the organic solvent to water or an aqueous solvent, where the volume of water or aqueous solvent is 5% or less of the volume of organic solvent; and collecting the water and detecting the presence of optical brighteners in the water via fluorescence. A preferable organic solvent is chloroform. Also claimed are: a kit for measuring the concentration of optical brighteners comprising cetyl trimethylammonium bromide; and the use of cetyl trimethylammonium bromide in a method or kit for measuring the concentration of optical brighteners in an environmental water source. Measurement of optical brighteners in fresh or sea water may be used to detect sewage contamination.

Description

(71) Applicant(s):
The Secretary of State for Defence (Incorporated in the United Kingdom) DSTL, Porton Down, Salisbury, SP4 0JQ, United Kingdom (72) Inventor(s):
Carl Nicholas Mayers (74) Agent and/or Address for Service:
DIPR Formalities Section
Poplar 2 #2214, MoD Abbey Wood (South), BRISTOL, BS34 8JH, United Kingdom (51) INT CL:
G01N 33/18 (2006.01) G01N 1/40 (2006.01)
G01N 21/64 (2006.01) (56) Documents Cited:
CN 105510112 A US 20150079692 A1
US 20110186753 A1
Water Research, vol. 43, 2009, Y. Cao et al., Evaluation of optical brightener photodecay characteristics for detection of human fecal contamination, pp. 2273-2279
Water Research, vol. 41, 2007, P. G. Hartel et al., Exposing water samples to ultraviolet light improves fluorometry for detecting human fecal contamination, pp. 3629-3642.
Journal of Chromatography A, vol. 1088, 2005, W-C Shu et al., Determination of fluorescent whitening agents in laundry detergents and surface waters by solid-phase extraction and ion-pair high-performance liquid, pp. 218-223.
Aldrich Chemistry Handbook of Fine Chemicals, 2012-2014, Sigma-Aldrich.
(58) Field of Search:
INT CL G01N
Other: WPI, EPODOC, CAS Online, XPESP, XPSPRNG, BIOSIS, MEDLINE, XPOAC, NPL, PUBCOMP, PUBSUBS, XPMISC, Internet (54) Title of the Invention: Method for measuring optical brighteners in environmental water Abstract Title: Method for measuring optical brighteners in environmental water (57) A method for measuring the concentration of optical brighteners in an environmental water source comprising: collecting a sample of water from an environmental source; adding to the sample an organic solvent that is immiscible with water, where the volume of the organic solvent is 5% or less of the volume of the water sample; adding to the water and organic solvent mixture cetyl trimethylammonium bromide as a detergent/phase-transfer agent and agitating the resultant mixture; allowing the water and organic solvent to re-separate following agitation and then removing the organic solvent from the mixture; adding the organic solvent to water or an aqueous solvent, where the volume of water or aqueous solvent is 5% or less of the volume of organic solvent; and collecting the water and detecting the presence of optical brighteners in the water via fluorescence. A preferable organic solvent is chloroform. Also claimed are: a kit for measuring the concentration of optical brighteners comprising cetyl trimethylammonium bromide; and the use of cetyl trimethylammonium bromide in a method or kit for measuring the concentration of optical brighteners in an environmental water source. Measurement of optical brighteners in fresh or sea water may be used to detect sewage contamination.
o □□ ho
Method for Measuring Optical Brighteners in Environmental Water
The present invention is concerned with improved methods for measuring the concentration of optical brighteners in water, especially in fresh or sea water as a measure of environmental contamination from sewage.
Optical brighteners are used to make paper, but also used in washing powder as a means of making laundry appear whiter: the optical brighteners improving the fluorescence under UV light. Typical optical brighteners used in washing powders include diaminostilbene dyes.
Waste (grey) water and sewage contain a high concentration of optical brighteners due to laundry waste water. Measuring the presence of optical brighteners in fresh or sea water is a common method to detect sewage contamination. This is usually achieved through sampling large volumes of water and measuring the concentration of optical brightener in those large volumes by fluorescence assay. Large volumes of water are required to be sampled because of the relatively low concentrations of optical brightener in the vast volumes of fresh and sea water on the planet.
Sampling large volumes of water is however time consuming and laborious. Improved methods are required to overcome the need to sample such large volumes of water.
The present application thus generally aims to overcome this problem, and provide methods that require smaller volumes of water for analysis of optical brighteners as a measurement of environmental contamination by sewage.
In a first aspect, the present invention provides a method for measuring the concentration of optical brighteners in an environmental water source sample comprising
i. collecting a volume of a sample of water from an environmental source, such as a river, a lake, or a sea;
ii. adding to the water a significantly smaller volume of an organic solvent, such as 5% or less of the volume of water, wherein the organic solvent is immiscible with the water;
ill. further adding to the water and organic solvent mixture the detergent cetyl trimethylammonium bromide, or a derivative thereof, and agitating the resulting mixture;
iv. allowing the water and organic solvent to re-separate following agitation, and then removing the organic solvent from the mixture;
v. adding to the organic solvent a significantly smaller volume of water, or alternatively an aqueous solvent, such as 5% or less of the volume of the organic solvent; and vi. removing the water and measuring the fluorescence of the optical brighteners in the water.
The Applicant has identified a new method by which to rapidly concentrate optical brighteners from a volume of water from an environmental source, such as a river, a lake or a sea.
It is generally known that optical brighteners are more soluble in water than in organic solvents, especially in organic solvents which are immiscible with water such as chloroform. The Applicant has however discovered that the detergent CTAB (cetyl trimethylammonium bromide) is able to act as a phase transfer catalyst for optical brighteners to allow them to move from an aqueous phase into an immiscible inorganic phase.
The organic solvent may be chloroform.
The concentration of the cetyl trimethylammonium bromide may be about 10 mM once added to the environmental water sample.
This chance discovery provides a very simple means to purify and greatly concentrate optical brighteners from environmental water sources.
In a second aspect, the present invention provides a kit for measuring the concentration of optical brighteners in an environmental water source sample, said kit comprising cetyl trimethylammonium bromide, or a derivative thereof.
In a third aspect, the present invention provides for use of cetyl trimethylammonium bromide, or derivatives thereof, in a method or kit for measuring the concentration of optical brighteners in an environmental water source.
The present invention shall now be discussed with reference to the following non-limiting example.
Example
In one experiment a large volume of seawater (multiple litres) comprising optical brighteners was placed in a flask, and cetyl trimethylammonium bromide (CTAB) added to a concentration of lOmM CTAB in the seawater. A small volume (e.g. 50 ml) of chloroform, although this could be other immiscible organic solvents, was added and the mixture agitated. The CTAB caused the optical brighteners in the seawater to partition from the aqueous (sea water) phase into the organic (chloroform) phase. The 50ml organic phase was removed to another flask, and 1 ml of water, which could also be an aqueous solvent, was added to it. Since the CTAB remained in the seawater, the optical brighteners were now able to partition into the smaller volume of water, and be measured/detected in that smaller volume of water. This process thus allows the optical brighteners in the environmental water sample to be concentrated from being in multiple litres of seawater into just a millilitre volume of water, thus enabling methods for measuring optical brighteners in environmental water samples to be more sensitive, but to also require much smaller volumes of the environmental water to be sampled.
The method has the potential to make the environmental screening of optical brighteners in the order of one thousand times more sensitive, using a cheap and commonly available reagent (CTAB) in a simple and fast protocol.

Claims (3)

  1. Claims
    1. A method for measuring the concentration of optical brighteners in an environmental water source sample comprising
    1. collecting a volume of a sample of water from an environmental source;
    ii. adding to the water a volume of an organic solvent immiscible with water, wherein the volume of the organic solvent is 5% or less of the volume of the sample of water from the environmental source;
    iii. further adding to the water and organic solvent mixture the detergent cetyl trimethylammonium bromide, or a derivative thereof, and agitating the resulting mixture;
    iv. allowing the water and organic solvent to re-separate following agitation, and then removing the organic solvent from the mixture;
    v. adding to the organic solvent a volume of water or a volume of an aqueous solvent, wherein the volume of the water or aqueous solvent is 5% or less of the volume of the organic solvent; and vi. removing the water to measure the fluorescence of the optical brighteners.
  2. 2. A kit for measuring the concentration of optical brighteners in an environmental water source sample, said kit comprising cetyl trimethylammonium bromide, or a derivative thereof.
  3. 3. Use of cetyl trimethylammonium bromide, or derivatives thereof, in a method or kit for measuring the concentration of optical brighteners in an environmental water source.
    Intellectual
    Property
    Office
    Application No:
    GB1814675.3
    Examiner:
    Dr Richard Wood
GB1814675.3A 2018-09-10 2018-09-10 Method for measuring optical brighteners in environmental water Withdrawn GB2576949A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
GB1814675.3A GB2576949A (en) 2018-09-10 2018-09-10 Method for measuring optical brighteners in environmental water

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB1814675.3A GB2576949A (en) 2018-09-10 2018-09-10 Method for measuring optical brighteners in environmental water

Publications (2)

Publication Number Publication Date
GB201814675D0 GB201814675D0 (en) 2018-10-24
GB2576949A true GB2576949A (en) 2020-03-11

Family

ID=63921291

Family Applications (1)

Application Number Title Priority Date Filing Date
GB1814675.3A Withdrawn GB2576949A (en) 2018-09-10 2018-09-10 Method for measuring optical brighteners in environmental water

Country Status (1)

Country Link
GB (1) GB2576949A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11079329B2 (en) * 2017-09-27 2021-08-03 University of North Carolina Wilmington Human waste water and human-derived pathogen scouting tool

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111458304B (en) * 2020-04-10 2023-04-18 海信冰箱有限公司 Fluorescent whitening agent detection system of washing machine
CN113834794A (en) * 2021-09-29 2021-12-24 浙江宏达化学制品有限公司 Detection method for rapidly detecting quality of fluorescent whitening agent

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110186753A1 (en) * 2010-02-02 2011-08-04 Mote Marine Laboratory, Inc. Method and apparatus for determining the presence of optical brighteners in water samples
US20150079692A1 (en) * 2013-09-19 2015-03-19 King Fahd University Of Petroleum And Minerals Method of determining phenoxy herbicides in water samples by phase transfer microextraction with simultaneous derivatization and gas-chromatography mass-spectrometry analysis
CN105510112A (en) * 2015-11-24 2016-04-20 长安大学 An aqueous two-phase system and applications thereof in enrichment of a trace fluorescent agent in a facial mask

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110186753A1 (en) * 2010-02-02 2011-08-04 Mote Marine Laboratory, Inc. Method and apparatus for determining the presence of optical brighteners in water samples
US20150079692A1 (en) * 2013-09-19 2015-03-19 King Fahd University Of Petroleum And Minerals Method of determining phenoxy herbicides in water samples by phase transfer microextraction with simultaneous derivatization and gas-chromatography mass-spectrometry analysis
CN105510112A (en) * 2015-11-24 2016-04-20 长安大学 An aqueous two-phase system and applications thereof in enrichment of a trace fluorescent agent in a facial mask

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Aldrich Chemistry Handbook of Fine Chemicals, 2012-2014, Sigma-Aldrich. *
Journal of Chromatography A, vol. 1088, 2005, W-C Shu et al., "Determination of fluorescent whitening agents in laundry detergents and surface waters by solid-phase extraction and ion-pair high-performance liquid", pp. 218-223. *
Water Research, vol. 41, 2007, P. G. Hartel et al., "Exposing water samples to ultraviolet light improves fluorometry for detecting human fecal contamination", pp. 3629-3642. *
Water Research, vol. 43, 2009, Y. Cao et al., "Evaluation of optical brightener photodecay characteristics for detection of human fecal contamination", pp. 2273-2279 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11079329B2 (en) * 2017-09-27 2021-08-03 University of North Carolina Wilmington Human waste water and human-derived pathogen scouting tool
US11828708B2 (en) 2017-09-27 2023-11-28 University of North Carolina Wilmington Human waste water and human-derived pathogen scouting tool

Also Published As

Publication number Publication date
GB201814675D0 (en) 2018-10-24

Similar Documents

Publication Publication Date Title
Al Amin et al. Recent advances in the analysis of per-and polyfluoroalkyl substances (PFAS)—A review
McDonough et al. Measuring total PFASs in water: The tradeoff between selectivity and inclusivity
Prasad et al. Solid phase extraction vis-a-vis coprecipitation preconcentration of cadmium and lead from soils onto 5, 7-dibromoquinoline-8-ol embedded benzophenone and determination by FAAS
GB2576949A (en) Method for measuring optical brighteners in environmental water
Gago-Ferrero et al. Liquid chromatography-tandem mass spectrometry for the multi-residue analysis of organic UV filters and their transformation products in the aquatic environment
Björklund et al. Fast extraction, clean-up and detection methods for the rapid analysis and screening of seven indicator PCBs in food matrices
Rastegarzadeh et al. Determination of trace silver in water, wastewater and ore samples using dispersive liquid–liquid microextraction coupled with flame atomic absorption spectrometry
Altunay Utility of ultrasound assisted-cloud point extraction and spectophotometry as a preconcentration and determination tool for the sensitive quantification of mercury species in fish samples
Dogruer et al. Effect-based approach for screening of chemical mixtures in whole blood of green turtles from the Great Barrier Reef
Cheng et al. Highly sensitive and selective detection of perfluorooctane sulfonate based on the Janus Green B resonance light scattering method
Liao et al. A simple, rapid and sensitive ultraviolet-visible spectrophotometric technique for the determination of ultra-trace copper based on injection-ultrasound-assisted dispersive liquid–liquid microextraction
Shao et al. Integrating bioassays, chemical analysis and in silico techniques to identify genotoxicants in surface water
Foltz et al. Simultaneous detection and quantification of select nitromusks, antimicrobial agent, and antihistamine in fish of grocery stores by gas chromatography–mass spectrometry
Liu et al. A graphene oxide-based fluorescence assay for the sensitive detection of DNA exonuclease enzymatic activity
Dey et al. FRET-based ‘ratiometric’molecular switch for multiple ions with efficacy towards real-time sampling and logic gate applications
Sasi et al. Alcohol ethoxysulfates (AES) in environmental matrices
Cantarero et al. Evaluation of the presence of major anionic surfactants in marine sediments
Escarrone et al. A vortex-assisted MSPD method for triclosan extraction from fish tissues with determination by LC-MS/MS
Liang et al. A ratiometric fluorescence recognition of guanosine triphosphate on the basis of Zn (II) complex of 1, 4-bis (imidazol-1-ylmethyl) benzene
JP5523324B2 (en) Detection of anionic surfactant
Ma et al. Simultaneous determination of nitroimidazoles and amphenicol antibiotics in water samples using ultrasound-assisted dispersive liquid–liquid microextraction coupled with ultra-high-performance liquid chromatography with tandem mass spectrometry
Usha et al. A graphene oxide-based fluorescent sensor for surfactants
Wufuer et al. Interaction of dissolved organic matter with Hg (II) along salinity gradient in Boston Lake
RU2283484C9 (en) Composition of standard samples for controlling error of measurements of oil products content in watery substances
Zhang et al. Sensitive determination of five priority haloacetic acids by electromembrane extraction with capillary electrophoresis

Legal Events

Date Code Title Description
WAP Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1)