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1、瓶口糖残留菲林试剂法操作配制SOPPrepared by/编制者：Reviewed by/审阅者：Authorized by/批准者：唐夏维品质保证总监吴晓文品质保证经理唐夏维品质保证总监Date/日期：Oct.19, 2003Date/日期：Oct.19, 2003Date/日期：Oct.19, 2003文件修改信息序号修改日期修改页数/纪要修改申请表序列号本文件最新修改日期： 年 月 日审批人：修改次数：第 次1 Objective目的：规范瓶口饮料残留定量测定的程序和方法，提供菲林试剂配置的标准程序，使检测结果真实有效。2 Scope范围：需要定量测定瓶口饮料残留的过程以及测定所需的菲林
2、试剂的配制过程3 Responsibility职责：品控测试人员负责执行该程序，品控经理对该程序执行的落实和监督负责。 4 Procedure程序：1. Cut the bottle in the middle and pour the beverage out. Pay attention to avoid beverage pouring to support ring and closure.1. 将瓶子从中间剪开，放掉饮料，注意不要让饮料流到瓶盖和支撑环处。2. Dry the upper part the bottle and open the closure while the c
3、losure is downward.2. 将剪开的瓶子的上半部分内外擦干净，瓶口向下，小心旋开。3. Dry the beverage at the top of bottle where is sealed by closure.3. 将瓶口顶端和瓶盖密封圈接触处的饮料小心擦干。4. Take Neck finish washing approximately 5ml4. 准备5毫升蒸馏水，对瓶口进行冲洗，目的是将瓶口螺纹处的饮料（如果有的话）用水带下来。将该5毫升水，反复淋洗瓶口螺纹5次，以确保将饮料全部带下。5. Using wash bottle collected by beake
4、r transfer to test tube5. 将上述的5毫升蒸馏水转到试管中。6. Acidify with 1 drop 1N HCl6. 向试管中滴入1滴1mol/L的盐酸，进行酸化。7. Heat to gentle boiling to prepare test sample of approximately 1ml7. 将试管缓慢加热到沸腾，使5毫升水蒸发到只有1毫升左右。8. It is necessary to first neutralize the HCl inverted sample. We use 1 drop 1N HCl per sample hence 1
5、drop 1N NaOH should suffice.8. 加入1滴1mol/L的氢氧化钠溶液，充分摇晃，使之反应完全。9. Add a drop of combined Fehling to test sample - heat to boiling9. 加入已经混合的菲林试剂1滴，到试管中。缓慢加热到沸腾。10. If Blue colour discharged - repeat Step 9 - until stable permanent blue10. 如果蓝颜色褪掉，重复步骤9，直到蓝颜色稳定不褪去。11. Record how many drops of combined F
6、ehling solution.11. 记录下共滴了多少滴菲林试剂。Remarks: Step 11 counts how many drops of Fehling solution to be neutralized. Then convert to volume. So please estimate the volume of one drop of water. (We take one drop as 0.05ml as usual) 另外，由于步骤11是统计菲林试剂滴了几滴，再转化为体积。故请先估算出每滴水的大概体积。（我们一般采用1滴为0.05ml）Stock Fehling
7、solution菲林试剂的配制：1. Dissolve 69.278 g copper sulphate (CuSO4.5H2O) in water and make up to 1 litre. (MW CuSO4.5H2O = 249.54)1. 配制菲林试剂1：溶解69.278 g (CuSO4.5H2O)于RO水中，并定容到1升。2. Dissolve 100 g sodium hydroxide and 346 g sodium potassium tartrate in water and make up to 1 litre.2. 配制菲林试剂2：溶解100 g 氢氧化钠和 34
8、6 g 酒石酸钠钾与RO水中，并定容到1升。3. Keep the Fehling solution 1 and 2 in the fridge.3. 将菲林试剂1和2保存在冰箱中。4. Mix each 25ml Fehling solution 1 and 2 to a brown glass bottle before production.4. 每次生产前，各取25ml菲林试剂1和2，混合入一棕色滴瓶中。5. Mixed Fehling solution can only use for the intraday production. Clean and dry the brown
9、glass bottle after production/5. 混合后的菲林试剂只能用于当天的生产，生产结束后，倒去未使用的菲林试剂，将棕色滴瓶洗干净并保持干燥。6 The Fehling solution 1 and 2 can be stored in fridge for at least 3 months.6. 冰箱中的菲林试剂1和2可以保存3个月。In off-season, preparation of Fehling solution 1 and 2 can reduce to 250ml to avoid wasting.在生产淡季，可考虑将菲林试剂1和2的配制减少到各250ml，以避免因过期而造成的浪费。Daily QC testing frequency日常品控测试频率1. A minimum sample of one round capper immediately after production startup.1. 开机，取样量为旋盖头的数量。2. Samples per hr until shutdown.3. 正常生产过程中，每小时取样2瓶，直到关机。Acceptable standard接受标准Accept =
