摘要
建立了在硝酸锶-乙二醇快速浸取后用电感耦合等离子体原子发射光谱法(ICP-AES)测定钢渣中游离氧化钙含量的方法。将研磨、过筛后的样品加热烘干,分取0.200 0 g,加入30 g·L^(-1)硝酸锶-乙二醇浸取剂30 mL,在80-90℃下磁力搅拌15 min,用于浸取样品中的总氧化钙,其中的Sr2+具有路易斯酸作用,能够加快乙二醇浸取氧化钙的速率。得到的溶液用乙二醇稀释至50 mL后,干过滤,分取5.00 mL滤液,用水定容至100 mL,按照优化的ICP-AES条件在393.366 nm处测定总氧化钙含量,以热重分析曲线中400-550℃间失重台阶对应的质量损失百分比,计算以氧化钙计的氢氧化钙含量,以二者之差计算游离氧化钙的含量。结果显示:氧化钙的质量浓度在100.0 mg·L^(-1)内与其对应的光谱强度呈线性关系,检出限(3s)为0.02 mg·L^(-1);对实际样品重复测定11次,所得测定值的相对标准偏差为0.68%-1.4%;加标回收率结果显示,氧化钙的回收率96.5%-102%。方法用于分析3个实际样品和一个水泥熟料标准样品,并同YB/T 4328-2012进行比对,所得的测定值与标准方法的测定值、标准样品的认定值基本一致。
A method for the determination of free calcium oxide in steel slag was established by inductively coupled plasma atomic emission spectrometry after rapid leaching with strontium nitrate-ethylene glycol.Sample was heated and dried after grinding and sieving,0.2000 g of sample was mixed with 30 mL of 30 g·L^(-1) strontium nitrate-ethylene glycol solution,thus to extract the total calcium oxide in the sample under magnetic stirring at 80-90℃for 15 min.Sr2+from of strontium nitrate-ethylene glycol solution had the efect of lewis acid,which could speed up the rate of ethylene glycol leaching calcium oxide.The solution obtained was diluted to 50 mL with ethylene glycol and dry filtered.An aliquot of 5.00 mL of the filtrate was diluted to 100 mL with water,the total calcium oxide content in which was determined at 393.366 nm under the optimized ICP-AES conditions.Based on the percentage of mass loss corresponding to 400-550℃weight loss steps in the TG curve,the content of calcium hydroxide in terms of calcium oxide was calculated,and the content of free calcium oxide could be obtained by the content difference between the total calcium oxide and calcium hydroxide.The results showed that linearity relationship between mass concentrations of calcium oxide and its corresponding spectral intensities was kept within 100.0 mg·L^(-1),with detection limit(3s)of 0.02 mg·L^(-1).The actual sample was repeatedly analyzed for 11 times and RSDs of the determined values were found in the range of 0.68%-1.4%.Results of the spiked recovery test ranged from 96.5%to 102%.The proposed method was used to analyze 3 actual samples and standard sample of acement clinker,and compared with YB/T 4328-2012,with the determined values obtained by this method basically the same as those obtained by the standard method and the certified value of standard sample.
作者
乌静
刘爱坤
杨菊蕾
WU Jing;LIU Aikun;YANG Julei(State Key Laboratory of Advanced Stainless Steel Materials,Taiyuan Iron&Steel(Group)Co.,Ltd.,Taiyuan 030003,China;Technology Center,Shanxi Taigang Stainless SteelCo.,Ltd.,Taiyuan 030003,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2021年第7期586-590,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
硝酸锶
乙二醇
浸取
电感耦合等离子体原子发射光谱法
游离氧化钙
钢渣
strontium nitrate
ethylene glycol
leaching
inductively coupled plasma atomic emission spectrometry
free calcium oxide
steel slag
