元素分析仪法测定凝固浴中二甲基亚砜
曹进喜1,赵德明1,宫汝燕1,王丹1,丛佳玥1,郭国建2
1.威海市计量所,山东威海 264200; 2.中国兵器工业集团第五三研究所,济南 250031
Determination of dimethyl sulfoxide in coagulation bath by elemental analyzer
曹进喜1,赵德明1,宫汝燕1,王丹1,丛佳玥1,郭国建2
1. Weihai metering technology research institute, Weihai 264200; 2. CNGC Institute 53, Jinan 250031, China
摘要:建立有机元素分析仪测定碳纤维纺丝用凝固浴中二甲基亚砜组分的方法。讨论了进样舟、样品质量、氧化温度、载气流量等参数对测试结果的影响,得到优化测试条件:选择与样品测试相同规格样品舟进行空白值的测定,样品取样质量为(2±0.2) mg,氧化温度为1ㄠ50℃,载气流量为200 mL/min,催化剂为氧化钨。6次平行测定结果的相对标准偏差为0.16%,方法的加标回收率为97.8%~102.9%。该方法具有取样量少、无需进行样品处理、快速方便等优点,可用于测定凝固浴体系中的二甲基亚砜。
Abstract:The composition of DMSO(dimethyl sulfoxide) in coagulation bath of carbon fiber spinning was determined by organic element analyzer. The influences of parameters such as injection boat, mass of sample, oxidation temperature and carrier gas flow on the test results were discussed, and the optimal test conditions were obtained. The blank value was determined by selecting the sample boat of the same specification as the sample test, the sample mass was (2±0.2) mg, the oxidation temperature was 1ㄠ50℃, the carrier gas flow rate was 200 mL/min, the catalyst was tungsten oxide. The relative standard deviation of the determination results was 0.16%(n=6), and the recoveries of the method were 97.8%-102.9%. The method has the advantages of less sample mass, no need for sample treatment, fast and convenient, which can be used for the determination of dimethyl sulfoxide in coagulation bath system.
关键词:元素分析仪;二甲基亚砜;硫含量;凝固浴
Keywords:element analyzer; dimethyl sulfoxide; sulfur content; coagulation bath
本文引用格式:
曹进喜,赵德明,宫汝燕,等.元素分析仪法测定凝固浴中二甲基亚砜[J].化学分析计量,2021,30(6):35.
Cao Jinxi,Zhao Deming,Gong Ruyan,et al. Determination of dimethyl sulfoxide in coagulation bath by elemental analyzer[J]. Chemical Analysis and Meterage,2021,30(6):35.
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