NL2026928B1 - NPE-free LSC cocktail compositions suitable for Low Level applications. - Google Patents

NPE-free LSC cocktail compositions suitable for Low Level applications. Download PDF

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NL2026928B1
NL2026928B1 NL2026928A NL2026928A NL2026928B1 NL 2026928 B1 NL2026928 B1 NL 2026928B1 NL 2026928 A NL2026928 A NL 2026928A NL 2026928 A NL2026928 A NL 2026928A NL 2026928 B1 NL2026928 B1 NL 2026928B1
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lsc
lsc cocktail
cocktail composition
branched
phosphate ester
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Canan Stomp-Smit Helena
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Perkinelmer Health Sciences B V
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/204—Measuring radiation intensity with scintillation detectors the detector being a liquid
    • G01T1/2042—Composition for liquid scintillation systems
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • High Energy & Nuclear Physics (AREA)
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  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Measurement Of Radiation (AREA)

Abstract

The invention relates to Liquid Scintillation Counting (LSC) cocktail compositions suitable for Low Level applications. It also relates to methods and uses related thereto. Provided is an LSC cocktail composition, preferably being free of nonylphenol ethoxylates (NPE’s), comprising (i) a solvent mixture comprising a Di—isopropylnaphtalene (DIN) isomer mixture and Tripropylene glycol ether; (ii) primary scintillator 2,5-Diphenyloxazole (PPO) and secondary scintillator 4-Bis(2-methylstyryl)benzene (Bis-MSB); and (iii) a mixture of non-ionic surfactants, preferably ethoxylated secondary alcohols, and an anionic surfactant, preferably a branched, ethoxylated phosphate ester.

Description

P126840NL00 Title: NPE-free LSC cocktail compositions suitable for Low Level applications.
The invention relates to Liquid Scintillation Counting (LSC) cocktail compositions suitable for Low Level applications. It also relates to methods and uses related thereto.
Background of the invention Liquid Scintillation Counting is a common analysis method in the field of radioactivity and one of the most widely used techniques for the detection of low-energy beta-emitting radioactive isotopes.
Use is made of an LSC cocktail, which absorbs the emitted energy and sends out photons that can be detected by a Photo Multiplier Tube (PMT). The radioactive decay energy excites the aromatic solvent, this energy 1s absorbed by the primary scintillator and emitted at a higher wavelength where the secondary scintillator absorbs the energy. During the decay from the excited state to the ground state, the scintillators produce photons that can be detected by the PMT. For a reliable measurement and a high efficiency, the sample should ideally dissolve in or form a stable, clear micro-emulsion with the LSC cocktail. In order to detect very low amounts of radiation (Low Level), an LSC cocktail preferably () produces a minimal amount of background noise, (i1) no reaction should take place between the LSC cocktail components and the sample and (ii) allows a large volume of sample to be added without causing phase separation. This requires a special LSC cocktail composition.
To acquire the highest possible efficiency, the LSC cocktail is composed of at least an aromatic solvent, primary scintillator and a secondary scintillator. This minimum composition is possible for organic, non-aqueous samples. For aqueous based samples an emulsifying LSC cocktail is required with an aromatic solvent, optionally a co-solvent, a primary scintillator, a secondary scintillator, a surfactant blend, mostly non-ionic with optional anionic surfactant, and optionally excipients such as preservatives.
The current LSC cocktails contain as solvent mainly the aromatics 1,2,4-Trimethylbenzene (Pseudocumene), Di-isopropylnaphthalene isomers (DIN) and Linear Alkyl Benzene (LAB). Commonly used co-solvents are Glycol ethers from the Diethylene glycol range such as Diethylene glycol monobutyl ether (Butyldiglycol), Diethylene glycol monomethyl ether (Methyldiglycol) and Diethylene Glycol Monoethyl Ether (Ethyldiglycol), but also mineral oils are used.
By far the most common used primary and secondary scintillators are respectively 2,5-Diphenyloxazole (PPO) and 1,4-Bis(2- methylstyryl)benzene (Bis-MSB). Other suitable scintillators are 2- biphenyl-4-yl-5-phenyl-1,3,4-oxadiazole (PBD), 2-(4-tert-butylphenyl)-5- (diphenylyl)-1,3,4-oxadiazole (Butyl-PBD), 1,4-bis(5-phenyloxazol-2- vDbenzene (POPOP) and 1,4-Bis(4-methyl-5-phenyloxazol-2-yl)benzene (Dimethyl-POPOP). These have the disadvantage of low solubility and high production cost.
The surfactants used in LSC cocktails are originally the non-ionic Nonylphenol Ethoxylates (NPE's), which have a positive effect on the efficiency due to the aromaticity, are good wetting agents and have excellent emulsifying and dispersing properties. NPE’s can be used in LSC cocktail compositions without issues in high concentrations. It is common to use a combination of different degrees of ethoxylation (EO chain length), for example a mix of 6EO, 7EO and 8EO. NPE’s originally were used extensively in laundry detergents, automotive and paints.
Besides non-ionic surfactants, anionic surfactants are frequently used, for instance sulfosuccinates. These compounds have the disadvantage of possible precipitation at higher concentrations. When an LSC cocktail is to be used for salt-containing samples, for example NaCl-solution or PBS buffer, it is common to add one or more anionic surfactants with phosphate functional groups to the composition. An aromatic Phosphate Ester is preferred due to the positive effect on the LSC cocktail efficiency.
Recently, the NPE's are scrutinized due to hormone disruptive properties of the breakdown products. Because of this, Alcohol Ethoxylates (AE’s) gained in popularity in the other user areas. Although AE’s are excellent wetting agents, their emulsifying and dispersing properties are moderate. Large amounts must be used, in combination with lack of aromaticity this results in a lower efficiency LSC cocktail. Especially within the field of Low Level applications this is an issue, where large amounts of sample in combination with a low-energy isotope such as Tritium must be determined. Typically, a 10 ml sample is mixed with 10 ml LSC cocktail to form a stable, clear micro- emulsion. The sample typically consists of 200 ml acidified drinking water, which is evaporated to 10ml sample. A high LSC cocktail efficiency is necessary to meet the detection limit. Due to the worldwide decreasing availability of NPE’s and the increasing demand for NPE substitutes, several NPE-free LSC cocktails have become commercially available for some years. However, an NPE-free LSC cocktail that is suitable for Low Level applications is still lacking due to the aforementioned disadvantage of low Tritium efficiency. The inventors therefore aimed at providing an LSC cocktail composition that is suitable for Low Level applications, and which is preferably free from NPE's.
Description of the invention It was found that the above goals can be met by the combined use of non- ionic surfactants not being NPE’s but rather AE’s, Propylene glycol ether co- solvent and a Phosphate Ester as anionic surfactant.
The moderate emulsifying and dispersing properties of AE’s translate in practice to a high required concentration, resulting in an LSC cocktail having a lower efficiency as compared to using NPE’s. However, when a combination is used of AE’s, Propylene glycol ether and a Phosphate Ester, it turns out the required concentration is increased only little, resulting in an LSC cocktail with sufficient efficiency for Low Level applications. The invention provides a Liquid Scintillation Counting (LSC) cocktail composition, preferably being free of nonylphenol ethoxylates (NPE’s), comprising: (1) a solvent mixture comprising a Di-isopropylnaphtalene (DIN) isomer mixture and Tripropylene glycol ether; (11) primary scintillator 2,5-Diphenyloxazole (PPO) and secondary scintillator 4-Bis(2-methylstyryl)benzene (Bis-MSB); and (im) a mixture of non-ionic surfactants, preferably ethoxylated secondary alcohols, and an anionic surfactant, preferably a branched, ethoxylated phosphate ester. In one embodiment, the LSC cocktail composition comprises the DIN mixture in an amount of 30-75% by weight, PPO in an amount of 0.1-1.5% by weight, and Bis-MSB in an amount of 0.01-0.3% by weight. In one embodiment, the LSC cocktail comprises Tripropylene glycol ether in an amount of 1-10% by weight.
In one embodiment, the LSC cocktail comprises alcohol ethoxylates (AEs), preferably AEs having a chain length of C11-C15.
In one embodiment, the LSC cocktail comprises AEs having different degrees of ethoxylation, preferably AEs having an ethoxylation degree (EO) that varies between 3EO and 12EQO.
5 In one embodiment, the LSC cocktail comprises AEs in an amount of about 20-55% by weight. In one embodiment, the LSC cocktail comprises a branched, ethoxylated phosphate ester having a chain length between C5-C10, and ethoxylation degree between 2EO-6EO.
In one embodiment, the LSC cocktail comprises a branched, ethoxylated phosphate ester in an amount of 5-15% by weight.
The invention also provides an LSC cocktail composition comprising Tripropylene glycol ether as a solvent, optionally in combination with a Di- isopropylnaphtalene (DIN) isomer mixture.
Still further, the invention provides an LSC cocktail composition comprising a branched, ethoxylated phosphate ester having a chain length of C5-C10 and an ethoxylation degree between 2EO-6EQ.
In one aspect, the invention provides a method of analyzing an aqueous sample by liquid scintillation counting, comprising contacting the sample with an LSC cocktail composition according to the invention, and measuring a light signal using a scintillation counter.
In one embodiment, the aqueous sample contains salt and/or an acid.
Also provided is the use of a branched, ethoxylated phosphate ester with chain length between C5-C10, and ethoxylation degree between 2EO-6EO, to increase the counting efficiency and/or to decrease the background signal of an LSC cocktail composition.
The AE’s are preferably secondary and ethoxylated. The Phosphate ester is preferably branched and ethoxylated. An additional advantage of a branched, ethoxylated Phosphate ester is the very low background, which is comparable or even lower than NPE containing LSC cocktails suitable for Low Level applications. Previously, it was found that neutralized Phosphate esters were required for a high efficiency and low background (Patent NL8303213). The consequent disadvantage is an acid-base reaction during LSC cocktail production, with heat formation causing discoloration and the requirement for an accurate pH determination. The extraordinary properties of the branched, ethoxylated Phosphate ester itself sustain a high efficiency and low background, eliminating the neutralization requirement, therefore no heat is formed during LSC cocktail production and there is no accurate pH requirement.
The aromatic solvent DIN can be present between 30-75% by weight. Besides the aromatic solvent, use of a co-solvent is necessary. In case of an NPE-free LSC cocktail suitable for Low Level applications, a Propylene glycol ether is preferred, more specifically a Tripropylene glycol ether. The co-solvent can be present in an amount of between 1-10% by weight.
In one aspect, the Tripropylene glycol ether is of the formula: R=H or R=CH,, withn=1-4 The primary scintillator 2,5-Diphenyloxazole (PPO) may be present in an amount of about 0.1-1.5% by weight. Secondary scintillator 1,4-Bis(2- methylstyryl)benzene (Bis-MSB) may be present in an amount of between about 0.01-0.3% by weight.
The non-ionic surfactants are preferably branched AE’s, with an aliphatic chain length in the range of C11-C15. The ethoxylation degree (EO) can vary between 3EO and 12EQO. The AEs may be present as a mixture in an amount of between 20-55% by weight.
In one embodiment, an LSC cocktail comprises C11-15 Ethoxylated secondary alcohols of the formula CH-(CH), CH-(CH), — CH, | | 0 | | | (CH,CH, 0) -H | mie HE | ¥ = peerage numberof ethylene oxide (EO grouss |
The anionic surfactant is preferably a branched, ethoxylated phosphate ester, with chain length between C5-C10 and ethoxylation degree between 2E0-6EO. It may be present in an amount of between 5-15% by weight. In one embodiment, the branched, ethoxylated phosphate ester is of the formula: CH, > (CH) — CH — {CH,),, — CH, | | CH2 | | | {CH,CH, 0), ~ 0 ~ POH, ; x= average mbar of ethylene oxide (ED groups |
EXAMPLES Table 1: Exemplary LSC cocktail composition according the invention [eee Di-isopropylnaphthalene (DIN) isomer 30-75 mixture Tripropylene glycol ether 2,5-Diphenyloxazole (PPO) 1,4-Bis(2-methylstyryl)benzene (Bis-MSB) 0.01 -0.3 C11-15 Ethoxylated secondary alcohol 20-55 Branched, ethoxylated Phosphate Ester 5-15 Table 2 shows the comparison between the existing NPE containing Ultima Gold® LLT (reference) and an LSC cocktail of the present invention. Samples were prepared in 20 ml HDPE vials with quick closure HDPE caps and consisted of 10 ml cocktail mixed with 10 ml of a demineralized water sample or without sample.
Samples were measured on a Tri-Carb 2910TR conditioned at 15°C with counting region 0.4-4.5 keV and quench indicator tSIE. Background measurements were performed in Low Level Count Mode with count time 200 minutes. Hereafter, samples were spiked with 10 nl of tritiated Myristic Acid in Toluene solution.
To compare instrument performance and sensitivity, the Figure of Merit (FOM) 1s the most widely used parameter in LSC. FOM is dimensionless with equation E2/B or E2V2/B, where E is the Efficiency in %, V the sample volume in ml and B the Background in cpm. When used for comparing LSC cocktail performance the instrument settings, count time and counting region are maintained equal.
SH Efficiency measurements were performed in normal Count Mode with a counting time of 30 minutes against either a custom prepared NPE-free quench curve for a cocktail of the invention or against a standard 3H Ultima Gold Quench curve for the Ultima Gold LLT reference.
Table 2: 3H Efficiency, background and FOM Sample:Cocktail | Cocktail | 3H Background | E2/ | E2V2 ratio (ml) Efficiency | (CPM) B /B (%) 0:10 Ultima 57.2 1.32 2487 | na Gold LLT 0:10 The 47.4 1.46 1536 | na invention 10: 10 Ultima 31.8 1.68 602 | 60193 Gold LLT 10: 10 The 23.8 1.97 289 | 28899 invention The sample load capacity of an NPE-free LSC cocktail of the invention for different types of samples was compared to that of the conventional NPE- containing Ultima Gold LLT (reference). The sample load capacity of an LSC cocktail is the amount (volume) of sample that can be added to give a stable, clear micro-emulsion. Table 3 shows the results for the sample load capacity at 20°C. Table 3: Sample load capacity comparison (ml sample per 10 ml LSC cocktail) Invention Ultima Gold LLT Demineralized 12 12 water Tap water Waldeck water Seawater [9 6
0.15M NaCl 2M HNO:

Claims (13)

CONCLUSIESCONCLUSIONS 1. Een Liquid Scintillation Counting (LSC) cocktailsamenstelling, bij voorkeur vrij van nonylfenolethoxylaten (NPE's), omvattende (1) een oplosmiddelmengsel dat een di-isopropylnaftaleen (DIN) 1somerenmengsel en tripropyleenglycolether omvat; (11) primaire scintillator 2,5-difenyloxazool (PPO) en secundaire scintillator 4-bis (2-methylstyryl) benzeen (Bis-MSB); en (iu) een mengsel van niet-ionogene oppervlakteactieve stoffen, bij voorkeur geéthoxyleerde secundaire alcoholen, en een anionogene oppervlakteactieve stof, bij voorkeur een vertakte, geëthoxyleerde fosfaatester.A Liquid Scintillation Counting (LSC) cocktail composition, preferably free of nonylphenol ethoxylates (NPEs), comprising (1) a solvent mixture comprising a diisopropylnaphthalene (DIN) isomer mixture and tripropylene glycol ether; (11) primary scintillator 2,5-diphenyloxazole (PPO) and secondary scintillator 4-bis(2-methylstyryl) benzene (Bis-MSB); and (iu) a mixture of nonionic surfactants, preferably ethoxylated secondary alcohols, and an anionic surfactant, preferably a branched, ethoxylated phosphate ester. 2. LSC-cocktailsamenstelling volgens conclusie 1, omvattende het DIN- mengsel in een hoeveelheid van 30-75 gew.%, PPO in een hoeveelheid van 0,1-1,5 gew.% en Bis-MSB in een hoeveelheid van 0,01-0,3 % op basis van gewicht.An LSC cocktail composition according to claim 1, comprising the DIN mixture in an amount of 30-75% by weight, PPO in an amount of 0.1-1.5% by weight and Bis-MSB in an amount of 0, 01-0.3% by weight. 3. LSC-cocktail volgens conclusie 1 of 2, omvattende tripropyleenglycolether in een hoeveelheid van 1-10 gew.%.An LSC cocktail according to claim 1 or 2, comprising tripropylene glycol ether in an amount of 1-10% by weight. 4. LSC-cocktailsamenstelling volgens een van de voorgaande conclusies, die alcoholethoxylaten (AE's) omvat, bij voorkeur AE's met een ketenlengte van C11- C15.An LSC cocktail composition according to any one of the preceding claims comprising alcohol ethoxylates (AEs), preferably AEs with a chain length of C11 -C15. 5. LSC-cocktailsamenstelling volgens conclusie 4, omvattende AE's met verschillende ethoxyleringsgraden, bij voorkeur AE's met een ethoxyleringsgraad (EO) die varieert tussen 3EO en 12EO.An LSC cocktail composition according to claim 4, comprising AEs with different degrees of ethoxylation, preferably AEs with a degree of ethoxylation (EO) ranging between 3EO and 12EO. 6. LSC-cocktailsamenstelling volgens conclusie 4 of 5, omvattende AE's in een hoeveelheid van ongeveer 20-55 gew.%.An LSC cocktail composition according to claim 4 or 5 comprising AEs in an amount of about 20-55% by weight. 7. LSC-cocktailsamenstelling volgens een van de voorgaande conclusies, omvattende een vertakte, geéthoxyleerde fosfaatester met een ketenlengte van C5-C10 en ethoxylermgsgraad van 2EO-GEO.An LSC cocktail composition according to any one of the preceding claims, comprising a branched, ethoxylated phosphate ester having a chain length of C5-C10 and an ethoxylate content of 2EO-GEO. 8. LSC-cocktailsamenstelling volgens een van de voorgaande conclusies, omvattende een vertakte, geëthoxyleerde fosfaatester in een hoeveelheid van 5- 15 gew.%.An LSC cocktail composition according to any one of the preceding claims comprising a branched, ethoxylated phosphate ester in an amount of 5-15 wt.%. 9. Een LSC-cocktailsamenstelling die tripropyleenglycolether als oplosmiddel omvat, eventueel in combinatie met een di-isopropylnaftaleen (DIN) isomerenmengsel.An LSC cocktail composition comprising tripropylene glycol ether as a solvent, optionally in combination with a diisopropylnaphthalene (DIN) isomer mixture. 10. Een LSC-cocktailsamenstelling die een vertakte, geéthoxyleerde fosfaatester omvat met een ketenlengte van C5-C10 en een ethoxyleringsgraad van 2EO-GEO.10. An LSC cocktail composition comprising a branched, ethoxylated phosphate ester having a chain length of C5-C10 and a degree of ethoxylation of 2EO-GEO. 11. Werkwijze voor het analyseren van een waterig monster door middel van vloeistofscintillatietelling, omvattende het in contact brengen van het monster met een LSC-cocktailsamenstelling volgens een van de conclusies 1-10, en het meten van een lichtsignaal met behulp van een scintillatieteller.A method of analyzing an aqueous sample by liquid scintillation counting, comprising contacting the sample with an LSC cocktail composition according to any one of claims 1-10, and measuring a light signal using a scintillation counter. 12. Werkwijze volgens conclusie 11, waarbij het waterige monster zout en / of een zuur bevat.The method of claim 11, wherein the aqueous sample contains salt and/or an acid. 13. Het gebruik van een vertakte, geëthoxyleerde fosfaatester met een ketenlengte tussen C5-C10 en een ethoxyleringsgraad tussen 2EO-6EO, om de telefficiëntie te verhogen en / of om het achtergrondsignaal van een LSC- cocktailsamenstelling te verlagen.13. The use of a branched, ethoxylated phosphate ester with a chain length between C5-C10 and a degree of ethoxylation between 2EO-6EO, to increase the counting efficiency and/or to decrease the background signal of an LSC cocktail composition.
NL2026928A 2020-11-19 2020-11-19 NPE-free LSC cocktail compositions suitable for Low Level applications. NL2026928B1 (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL8303213A (en) 1983-09-16 1985-04-16 Packard Becker Bv MIXTURE FOR APPLICATION IN LSC (LIQUID SCINTILLATION COUNTING) ANALYSIS TECHNIQUE.
US4657696A (en) * 1984-09-19 1987-04-14 Fisons Plc Scintillation counting medium and counting method
JPH08166459A (en) * 1994-06-08 1996-06-25 Packard Instr Bv Scintillation counting system using scintillation capsule
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Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL8303213A (en) 1983-09-16 1985-04-16 Packard Becker Bv MIXTURE FOR APPLICATION IN LSC (LIQUID SCINTILLATION COUNTING) ANALYSIS TECHNIQUE.
US4657696A (en) * 1984-09-19 1987-04-14 Fisons Plc Scintillation counting medium and counting method
US4657696B1 (en) * 1984-09-19 1991-05-28 Scintillation counting medium and counting method
JPH08166459A (en) * 1994-06-08 1996-06-25 Packard Instr Bv Scintillation counting system using scintillation capsule
WO2003062350A1 (en) * 2002-01-07 2003-07-31 Packard Bioscience B.V. Liquid scintillation counting
US9274237B2 (en) * 2013-07-26 2016-03-01 Lawrence Livermore National Security, Llc Lithium-containing scintillators for thermal neutron, fast neutron, and gamma detection
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Title
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