摘要
称取羧甲基淀粉钠样品(0.50g左右),加超纯水定容至100mL,摇匀,静置。取上清液过反相固相萃取柱,弃去先流出液3mL,收集其后流出液2mL(供测定Cl-离子用的试液需再次稀释10倍),供色谱分析。选用SH-AC-4型阴离子交换柱(250mm×4.6mm)进行色谱分离,以2.4mmol·L^(-1)碳酸钠-6.0mmol·L^(-1)碳酸氢钠溶液为流动相,用抑制型电导检测器测定。所测5种阴离子均在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)为0.027,0.020,0.007 0,0.16,0.022 mg·L^(-1)。方法用于羧甲基淀粉钠样品的分析,加标回收率在88.3%~108%之间,测定值的相对标准偏差(n=5)在0.68%~11%之间。
A portion of the sample （around 0. 50 g） was mixed with water and the volume of the mixture was made up to 100 mL. After mixing and standing, the supernatant was taken and passed through RP-SPE column. The first 3 mL of the effluent were discarded and the next 2 mL were collected as sample solution for IC analysis. For use in determination of Cl^--ion, the effluent should be diluted 10 times. SH-AC-4 anion exchange column （250 mm×4. 6 mm） was used for IC separation, and mixed solution of 2. 4 mmol ·L^-1 Na2CO3-6. 0 mmol ·L^-1 NaHCO3 was used as mobile phase. Restrain conductance detector was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 5 anions were kept in definite ranges. Detection limits （3S/N） found were 0. 027, 0. 020, 0. 007 0, 0. 16, 0. 022 mg ·L^-1 respectively. The proposed method was applied to the analysis of substantial sample and recovery was tested by standard addition method giving values of recovery in the ranges of 88. 3%-108% and values of RSD＇s （n=5） were found in the range of 0. 68%- 11%.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第5期611-614,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
