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1. 绘制环氧乙烷标准曲线
1.1 标准溶液的制备
取外购环氧乙烷标准液1支(约1ml),用移液器吸取全部的EO标准液置已去皮的50ml容量瓶(已加水30ml)中,精密称定0.9980g,再加水至刻度,摇匀,即得99.7840μg/mL环氧乙烷标准贮备液。再稀释制备1μg/ml-10μg/ml六个系列浓度的标准溶液(实际浓度为0.9978μg/ml、2.9935μg/ml、4.9892μg/ml、6.9849μg/ml、8.9806μg/ml、9.9784μg/ml)。
1.2 进样及绘制标曲
精确量取上述各浓度标准溶液各5ml,分别置20ml顶空瓶中,密封,恒温(60℃±1℃)中平衡40min。依次进样,记录环氧乙烷峰面积,绘制标曲(见附件 )。
2.样品试液制备
取2个最小包装的样品,分别称取样品①1065_g、②1.1876_g,加入纯化水5ml,振摇, /℃浸提一小时。
3.样品测试
分别量取5ml样液置20ml顶空瓶中,密封,置顶空进样器中60℃±1℃平衡40min,再1ml进样检测,记录峰面积。(图谱见附件 )。
4.含量计算
计算公式:试样EO浓度X=(Y-b)/a(X:EO浓度μg/mL,Y:峰面积)样品EO含量(μg/g)=试样E0浓度(μg/ml)×稀释体积(m1)/样品质量(g)结果为人咕 _ug/g(计算过程见附件 )
5.检出限测定
当样品未检出环氧乙烷时,应进行检出限的测定:
取( )/μg/ml环氧乙烷标准溶液,稀释( )倍(浓度为( μg/ml)后,进样测试,记录峰高值(I)( ),噪音值(N)( )。(图谱见附件 )
计算:检出限D=3×C/(I/N)×V/m 结果:
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