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Determination of sodium and potassium contents in palm-based polyols using graphite furnace atomic absorption spectrometer
Chemical Papers ( IF 2.1 ) Pub Date : 2021-01-20 , DOI: 10.1007/s11696-020-01493-8
Nur Aainaa Syahirah Ramli , Mohd Azmil Mohd Noor , Tuan Noor Maznee Tuan Ismail

In the production of palm-based polyols (PBP), multiple purification steps might introduce sodium (Na) and potassium (K) into the polyols. The Na and K have potential to influence reactivity of polyether polyols with isocyanate in polyurethane (PU) production. The Na and K contents in polyether polyols for PU production are both limited to 10 mg kg−1. This study focuses on method(s) development for determination of Na and K in PBP by graphite furnace atomic absorption spectrometer (GF AAS) using dilution in isopropyl alcohol as a sample preparation method. All measurements were performed without any chemical modifier. In GF AAS analysis, it is essential to establish the optimum temperature program which includes pyrolysis and atomization temperature. At the optimized condition, the developed method was validated according to the validation protocol described by International Conference on Harmonization (ICH) and AOAC International. Several parameters were evaluated include linearity of calibration curve, limit of detection (LOD), limit of quantitation (LOQ), sensitivity, recovery, and precision. The optimization of temperature program for both Na and K determinations deduced the optimum pyrolysis and atomization temperature of 900 and 1600 °C, respectively. The method for Na determination concludes as follows: the analytical curve showed linear correlation with R2 value of 0.9928. The LOD and LOQ were 0.307 and 1.025 µg kg−1, respectively. Recoveries in the range of 97 to 108% were obtained from spiked samples (4–12 µg kg−1). Whereas, the method for K determination deduces as follows: the analytical curve showed linear correlation with R2 value of 0.9985. The LOD and LOQ were 0.249 and 0.829 µg kg−1, respectively. Recoveries in the range of 90–109% were obtained from spiked samples (4–12 µg kg−1). The Na and K contents obtained from the developed GF AAS method are in agreement with inductively coupled plasma optical emission spectrometry (ICP OES) with 95% confidence level. The Na and K contents in PBP samples were within the limit allowed for PU production.



中文翻译:

用石墨炉原子吸收光谱仪测定棕榈基多元醇中的钠和钾含量

在棕榈基多元醇(PBP)的生产中,多个纯化步骤可能会将钠(Na)和钾(K)引入多元醇中。Na和K有可能影响聚氨酯(PU)生产中聚醚多元醇与异氰酸酯的反应性。用于生产聚氨酯的聚醚多元醇中的Na和K含量均限制为10 mg kg -1。这项研究的重点是通过使用异丙醇稀释作为样品制备方法的石墨炉原子吸收光谱仪(GF AAS)测定PBP中的Na和K的方法。所有测量均在没有任何化学改性剂的情况下进行。在GF AAS分析中,必须建立包括热解和雾化温度在内的最佳温度程序。在最佳条件下,根据国际协调会议(ICH)和AOAC International描述的验证协议对开发的方法进行了验证。评估了几个参数,包括校准曲线的线性,检测限(LOD),定量限(LOQ),灵敏度,回收率和精密度。用于Na和K测定的温度程序优化分别推导了900和1600°C的最佳热解和雾化温度。钠的测定方法总结如下:分析曲线与R 2值为0.9928。LOD和LOQ分别为0.307和1.025 µg kg -1。从加标样品(4–12 µg kg -1)中回收率在97%至108%之间。而测定K的方法推导如下:分析曲线显示线性相关,R 2值为0.9985。LOD和LOQ分别为0.249和0.829 µg kg -1。从加标样品(4–12 µg kg -1)中回收率在90–109%范围内)。从发展的GF AAS方法获得的Na和K含量与电感耦合等离子体发射光谱法(ICP OES)具有95%的置信度。PBP样品中的Na和K含量在PU生产允许的范围内。

更新日期:2021-01-20
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