离子色谱法测定芳香族聚酰胺纤维中硫、钠、钾、钙、镁  

ION-CHROMATOGRAPHIC DETERMINATION OF SULFUR SODIUM POTASSIUM MAGNESIUM AND CALCIUM IN AROMATIC POLYAMIDE FIBER

作　　者：王少明[1] 荀其宁[1] 王爱萍[1] 于乃海[2] 

机构地区：[1]中国兵器工业集团五三研究所,济南250031 [2]山东电力研究院,济南250002

出　　处：《理化检验（化学分册）》2006年第3期176-178,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

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。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 Na2 CO3 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 SO4^2-, Na^＋ , K^＋, Mg^2＋ and Ca^2＋ were found as 0. 02, 0. 25, 0. 25, 0. 70 and 0. 80 mg· L^-1 respectively.

关 键 词：离子色谱法 硫 钠 钾 镁 钙 芳香属聚酰胺纤维 

分 类 号：O657.7[理学—分析化学]