【摘要】 应用离子色谱法(IC)测定芳香族聚酰胺纤维中硫、钠、钾、镁及钙。测定阴离子时,试样置于铂坩埚中用艾斯卡试剂覆盖,置于马弗炉中,450℃灼烧1 h使有机物碳化,取出,稍冷,再加少许艾斯卡试剂,升温至850℃灼烧1．5 h,使有机物完全分解。坩埚中的熔块经冷却后用去离子水浸出,用18 mmol·L-1碳酸钠及17 mmol·L-1碳酸氢钠混合溶液定容后,用IC法的阴离子方式测定。用IC法测定阳离子时,试样置于铂坩埚中,不必加艾斯卡试剂,置于马弗炉直接灼烧至有机物完全分解。残渣用1 mol·L-1硝酸或1 mol·L-1盐酸超声波处理,用去离子水洗涤坩埚并定容至100 mL,按所测得峰面积值从标准曲线查得其含量。用此方法测定SO42-,Na+,K+,Mg2+及 Ca2+的检出限依次为0．02,0．25,0．25,0．70及0．80 mg·L-1。更多还原

【Abstract】 Ion chromatography (IC) was applied to the determination of some inorganic elements in aromatic polyamide fiber (Twaron). For the determination of anions, the sample in a platinum crucible was covered with Eschka mixture containing 3 parts of anhydrous Na2CO3 and 2 parts of zinc oxide, and heated in a muffle furnace at 450℃ for 1 h, some more of the Eschka mixture was added and heated at 850℃ for 1. 5 h, to decompose the organic substance completely. The cooled melt in the crucible was dissolved in deionized water, and diluted to 100 mL in a volumetric flask with a mixed solution containing 18 mmol·L-1 Na2CO3 and 17 mmol·L-1 NaHCO3. This sample solution was used for IC determination of anions. For the IC-determination of cations (e. g.alkali metal and alkaline earth metal ions), the sample in the crucible was burned directly in a muffle furnace, without adding the Eschka mixture, until complete oxidation of the organic substances was attained.The residue in the crucible was treated ultrasonically with 1 mol·L-1 HNO3 or 1 mol·L-1 HCl,and transferred to a 100 mL volumetric flask, wash the crucible and diluted to 100 mL with deionized water. Working conditions of the IC determination were described, and the results of the 5 elements were found by the standard curve method.Detection limits for SO42-, Na+ , K+ , Mg+ and Ca2+ were found as 0. 02, 0. 25, 0. 25, 0. 70 and 0. 80 mg·L-1 respectively.更多还原