活性炭管中乙酸乙酯、乙酸丁酯标准物质的研制

Development of certified reference materials for ethyl acetate and butyl acetate in activated carbon tubes

目的 研究活性炭管介质中乙酸乙酯、乙酸丁酯标准物质的制备,用于对工作场所中乙酸乙酯、乙酸丁酯样品量值的溯源及质量控制。方法 采用向活性炭管中直接加入标准溶液的方法制备高低2个浓度的标准样品。通过气相色谱法对样品进行分析,对乙酸乙酯、乙酸丁酯标准物质的均匀性、稳定性及定值引入的不确定度进行评估。结果 活性炭管介质中乙酸乙酯低、高2个浓度样品相对标准偏差(relative standard deviation,RSD)为1.1%、1.4%,乙酸丁酯低、高2个浓度样品RSD为1.4%和1.7%,RSD均<3%,活性炭管介质中乙酸乙酯、乙酸丁酯具有良好的均匀性,在4℃冷藏条件下可以稳定保存5个月,5~9个月间测量结果出现明显下降,下降率约为20%;通过对标准物质进行定值分析,乙酸乙酯标准物质量值水平:低浓度为(307.0±13.4)μg,高浓度为(629.0±38.2)μg;丁酯标准物质量值水平:低浓度为(319.5±20.6)μg,高浓度为(638.5±37.6)μg。结论 活性碳管中乙酸乙酯、乙酸丁酯标准物质在冷藏条件保存下可用于职业卫生样品检测、质量控制、量值溯源及分析方法的研究。

Objective To study the development of ethyl acetate and butyl acetate reference materials in activated carbon tube media,which is used for traceability and quality control of ethyl acetate and butyl acetate in the workplace.Methods The standard samples with high and low concentrations were prepared by directly adding standard solution into activated carbon tube.The homogeneity,stability and uncertainty introduced by fixed values of ethyl acetate and butyl acetate reference materials were evaluated by gas chromatography analysis of the samples.Results The relative standard deviation(RSD)of low and high concentration of ethyl acetate samples in activated carbon tube media was 1.1%and 1.4%respectively,and the RSD of low and high concentration of butyl acetate was 1.4%and 1.7%respectively.The RSDs were all<3%,and the ethyl acetate and butyl acetate in the activated carbon tube have good uniformity and can be stored for five months under 4 C cold storage condition.The measured results showed a significant decrease in 5-9 months,with a decrease rate of about 20%.The calibration analysis on reference materials was conducted,the quality value level of the ethyl acetate standard material was(307.0+13.4)μg at low concentration and(629.0±38.2)μg at high concentration,and the quality value level of butyl acetate standard material was(319.5±20.6)μg at low concentration and(638.5+37.6)μg at high concentration.Conclusion The ethyl acetate and butyl acetate reference materials in activated carbon tubes stored under refrigeration conditions can be used in quality control,traceability and analysis of occupational hygiene samples.