主题:【讨论】关于参考加拿大标准测试重金属的前处理问题

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xyq_lg2005
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最近主管组织对作业指导书进行修改,发现有一个问题,如下:
旧作业指导书 参考标准 Canada Hazardous Products Act R.S.C.1985, c.H-3 Schedule I Part I Item9
样品处理:准确称取样品0.2g,精确至0.0001g。用c(HCl)等于5.0%(v/v)的盐酸溶液25ml与测试试样混合,使混合物避光,在温度为20℃时搅拌混合物10分钟。接着立刻将混合物中的固体物有效分离出来,先使用中速定性滤纸预过滤,再用孔径为0.45μm滤膜过滤器过滤,收集滤液于锥形瓶中。

现加拿大测试重金属标准最新版本为:

Canada Consumer Products Safety Act SOR/2011-17 第23节
样品处理大概步骤:
Method C03中
4.2 Transfer the removed coating to a mortar and grind the sample with a pestle. An electric grinder may be used when the sample is too difficult to grind with apestle and a mortar. Sieve the ground coating with a 500 :m sieve. The
sample passing through the 500 :m sieve is then sieved through a 250 :msieve. The portion of the ground coating that passes the 500 :m and does not
pass the 250 :m is used for the leaching test. Place the sieved portion in a
weighing vessel and dry to constant weight (to the nearest 1 mg) in an air
convection oven at 60°C ± 3°C. This may take about an hour. Record the drying
time in the oven Log book and on the Results of Analysis data sheet. Remove
the vessel from the oven and cool in a desiccator.
4.5 Dried coating
4.5.1 Transfer about 100 mg of the dried coating into a tared 100 mL beaker
and weigh to the nearest 0.1 mg. Add 20 mL of the 5% (v/v) HCl
leaching solution and immediately start stirring for 10 ± 1 minutes at
20°C ± 3°C with the use of digital shaker (speed 140) or a magnetic
stirrer. At the end of the 10 ± 1 minutes, immediately filter the solution
through a Whatman no. 40 filter paper in a funnel, into a 50 mL
volumetric flask or certified 50 mL sample tube. Wash with a few mL of
ultra-pure water, add 1 mL of concentrated nitric acid, and make up to
volume with ultra-pure water. At least three replicate analyses should
be performed on each coating sample.
4.9 Dilute the worked-up leachate solutions prepared in sections 4.5, 4.6, 4.7 ten times using 2% (v/v) nitric acid.


称取通过0.5mm而不通过0.25mm金属筛网的样品0.1g,加入20ml 5%HCLV/V)与样品混合,在温度为20时搅拌混合物10分钟,接着立刻将混合物中的固体物有效分离出来,加入1ml硝酸,用纯净水定容至50ml。然后再把溶液稀释10倍,用2%硝酸定容,待测。
请问大家:现在修改作业指导书是不是要完全按标准上写的去做啊?以前的同事编写的作业指导书好像有好多都跟标准不是很一致,这样也符合吗?如果是被CNAS的专家来现场评审,这个算不算很严重的不符合项呀?
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依风1986
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Fe
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我是直接萃取后过滤了就上机分析了。没有加硝酸定容
Fe
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专家不会看这个的吧,你可以做个方法比较啊,到时给专家看如果没有差异的话应该问题不大啊,严格按照这个做每天几百个怎么做啊
小鬼当家
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称取通过0.5mm而不通过0.25mm金属筛网的样品0.1g,加入20ml 5%HCL(V/V)与样品混合,在温度为20℃时搅拌混合物10分钟,接着立刻将混合物中的固体物有效分离出来,加入1ml硝酸,用纯净水定容至50ml。然后再把溶液稀释10倍,用2%硝酸定容,待测。
加拿大的标准一直都要求这样做的啊,1985年太旧了吧,操作规程肯定要跟标准,即便这样还要做方法确认,确认你们实验室有能力做这个方法,现场评审时一定按标准做,不能有侥幸心理
liu999999
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