Identification of polymer additives by liquid chromatography–mass spectrometry

Block, Chantal; Wynants, Luc; Kelchtermans, Mauritz; Boer, R De; Compernolle, Frans

doi:10.1016/j.polymdegradstab.2006.07.015

Cited by 45 publications

(34 citation statements)

References 8 publications

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“…The development of new ionization techniques promoted MS for highly sensitive and selective detection [10,[20][21][22]24]. Compared with MS, IR detection lost its importance [23].…”

Section: Chromatographic Procedures For Stabilizersmentioning

confidence: 99%

Analysis of polyolefin stabilizers and their degradation products

Reingruber

Buchberger

2010

J of Separation Science

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Polymeric materials are complex samples, as they contain various groups of additives, compounding ingredients, and fillers. An important group of additives are stabilizers. Efficient stabilization is essential especially for polypropylene, as it is sensitive to oxidation and radical attack due to the numerous tertiary carbon atoms in its structure. How long a polymer will be sufficiently stabilized can be deduced from the contained amount of intact stabilizer. Different approaches for the analysis of stabilizers in polyolefins are available, which include sample preparation with subsequent chromatographic separation as well as direct analysis techniques. In round-robin tests, stabilizer concentrations obtained varied strongly. This shows the demand for reliable and robust methods. Stabilizers get consumed while protecting the polymer and are then present as degradation products. They were observed while quantifying intact stabilizers, in migration studies, and - if volatile - in emission studies of polymers. Furthermore, e.g. interactions with other polymer ingredients or irradiation degraded stabilizers. The identification of degradation products provides a better insight into the reactions associated with stabilization. Their quantitation makes it possible to deduce the original level of stabilization. Furthermore, polymer ingredients degrading stabilizers can be identified. Knowledge on these interactions contributes significantly to improved polymer stabilization.

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“…The development of new ionization techniques promoted MS for highly sensitive and selective detection [10,[20][21][22]24]. Compared with MS, IR detection lost its importance [23].…”

Section: Chromatographic Procedures For Stabilizersmentioning

confidence: 99%

Analysis of polyolefin stabilizers and their degradation products

Reingruber

Buchberger

2010

J of Separation Science

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“…For the highest molecular mass additives such as Irganox 1010 (MW [ 1000 mol g -1 ), other authors [155][156][157][158] tested ionization suitability using different desorption ionization techniques and highlighted that in the case of additives mixtures, the difference in ionization of the components must be taken into account.…”

Section: Degradation Of the Additivesmentioning

confidence: 99%

Physico-chemical ageing of ethylene–norbornene copolymers: a review

et al. 2017

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The main object of this report is to review and summarize the current state of the scientific literature relating to physico-chemical ageing of ethylene-norbornene copolymers (ENCs). These processes occur through different means such as photodegradation under the effect of ultraviolet radiation, temperature and ionizing radiation (under air or oxygen). In most cases ageing causes chains scissions that lead to the creation of degradation compounds that exhibit high mobility, corresponding to their low molecular weight and/or high polarity. Cross-linking can also occur, leading to the modification of mechanical properties. The presence of oxygen during ageing is of great importance for the physico-chemical modifications of those polymers in terms of oxidation and thermal stability. ENCs belong to cyclic olefin copolymers (COC) class, whose synthesis was developed in the late 1950s. Nevertheless, commercial applications are relatively new. They attract growing interest in different fields, due to their very useful physical and chemical properties such as transparency, heat and chemical resistance, low permeability to gas as well as biocompatibility. In the literature, a large number of papers deal with the synthesis and characterization of different grades of ENC, but only a few deal with the effects of ageing on these materials. This literature review consists of a summary of the main milestones in the development of COC as well as of cyclic olefin polymers (COP), a review of main techniques for predicting ageing, degradation of additives and interaction between COC/COP and contact environment as well as toxicity of the extractables.

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“…Although high-performance liquid chromatography (HPLC) is a very good method for the separation of complex additives, there are some difficulties in the identification of some components. [8][9][10][11] Gas chromatography coupled with mass spectrometry (GC-MS) is very beneficial for separating and identifying some additives, but when dealing with antioxidants and stabilizers it is not feasible in many cases, owing to their decomposition or lack of volatility. Only a few papers have been published concerning determination of some additives.…”

mentioning

confidence: 99%

Determination of Calcium Stearate in Polyolefin Samples by Gas Chromatographic Technique after Performing dispersive Liquid-Liquid Microextraction

2008

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The extraction and subsequent separation and quantification of polymer additives in polyolefins have proven to be a challenge for analytical chemists. [1][2][3][4][5][6][7] The quantification of additives in polymers is important in forensic investigations, scientific research and quality control. Currently, a range of additives is being used for protection during processing, increasing the lifetime and improving the performance of products. Although high-performance liquid chromatography (HPLC) is a very good method for the separation of complex additives, there are some difficulties in the identification of some components. [8][9][10][11] Gas chromatography coupled with mass spectrometry (GC-MS) is very beneficial for separating and identifying some additives, but when dealing with antioxidants and stabilizers it is not feasible in many cases, owing to their decomposition or lack of volatility. Only a few papers have been published concerning determination of some additives. Pyrolysis-GC, which needs to special instrument, is a common technique for this purpose. [12][13][14][15][16][17][18] So far, calcium stearate, which is added to polyolefins as a lubricant, was not directly determined by chromatographic techniques. It has a limited solubility in organic solvents, especially in those solvents that are used as a mobile phase or a modifier in liquid chromatography. On the other hand, calcium stearate cannot be determined by a gas-chromatographic technique due to its low volatility. In this study a gas chromatographic technique was presented for the determination of calcium stearate in polyolefin samples after its conversion to stearic acid.A recently presented extraction technique, dispersive liquid-liquid microextraction (DLLME), [19][20][21] was used to preconcentrate the analyte before its injection to GC. In this method, a solvent with a density higher than that of water at the range of microliter is used as an extracting solvent. Another solvent, such as methanol, acetonitrile, tetrahydrofuran or acetone which is miscible with both aqueous and organic solvents is added as a dispersive agent to disperse the extracting solvent into the aqueous phase. DLLME is a rapid and efficient extraction technique. It uses an extraction solvent at the mL level. In DLLME, a higher enrichment factor is achievable compared with ordinary liquid-liquid extraction techniques. experimental ApparatusA gas chromatograph STG Model GC 101B (Teif Gostar Co., Tehran, Iran), equipped with a flame ionization detector (FID), was used. The injection port system was a spilt/splitless injector. The characteristics of the capillary column and the GC conditions used in this analysis were as follows: column, Optima-1 (1.5 m ¥ 0.25 mm i.d.); thickness of stationary phase, 0.1 mm (Macherery Nagel, Germany); average linear velocity of nitrogen as carrier gas, 30 cm s -1 ; flow-rate of nitrogen as make up gas, 35 mL min -1 ; flow-rate of air and hydrogen for FID flame, 300 and 35 mL min -1 , respectively; temperature of the injection port, 200˚...

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Identification of polymer additives by liquid chromatography–mass spectrometry

Cited by 45 publications

References 8 publications

Analysis of polyolefin stabilizers and their degradation products

Analysis of polyolefin stabilizers and their degradation products

Physico-chemical ageing of ethylene–norbornene copolymers: a review

Determination of Calcium Stearate in Polyolefin Samples by Gas Chromatographic Technique after Performing dispersive Liquid-Liquid Microextraction

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