主题：【求助】对于ccpsa 测玩具中可溶Ba,Se的前处理程序的疑问

原文由 sega741(sega741) 发表:

原文由 燕飞(mansonyang) 发表:

原文由 sega741(sega741) 发表:
另在哪个部分讲到称样量和加5%HCL体积的啊

测试部分是与之前的CHPA一样的，操作看回之前的方法

CHPA现行有效的标准号是什么啊

可溶部分参考加拿大的C03

其实很简单，我们做的时候是加冰块或者是用冷却循环水的水做的，温度是控制在20+/-2度，，称样0.1g,加5ml的5%HCL(VHCL/VH200,振荡10分钟，然后定容50ml,定容前加1ml硝酸，样品要过0.25mm的分子筛

附C-03标准.
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 a pestle and a mortar.
Sieve the ground coating with a 500 :m sieve. The sample passing the 500 :m is then
sieve through a 250 :m. The portion of the ground coating that passes the 500 :m and
do not pass the 250 :m is used for the test. Place the portion in a weighing vessel and
dry to constant weight (to the nearest 1 mg) in an air convection oven at 60OC for 1 hour
Remove the vessel from the oven and cool in a desiccator.
4.3 Accurately transfer 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 min at 20 ± 2°C with the use of an oscillating hotplate or a
magnetic stirrer. Filter the solution, with a filter paper Whatman no.40 and a glass
funnel, into a 50 mL centrifuge tube, wash with a few mL of deionized water, add 1 mL
of concentrated nitric acid, and make up to volume with deionized water.

原文由 依风1986(xurunjiao5339) 发表:
附C-03标准.
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 a pestle and a mortar.
Sieve the ground coating with a 500 :m sieve. The sample passing the 500 :m is then
sieve through a 250 :m. The portion of the ground coating that passes the 500 :m and
do not pass the 250 :m is used for the test. Place the portion in a weighing vessel and
dry to constant weight (to the nearest 1 mg) in an air convection oven at 60OC for 1 hour
Remove the vessel from the oven and cool in a desiccator.
4.3 Accurately transfer 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 min at 20 ± 2°C with the use of an oscillating hotplate or a
magnetic stirrer. Filter the solution, with a filter paper Whatman no.40 and a glass
funnel, into a 50 mL centrifuge tube, wash with a few mL of deionized water, add 1 mL
of concentrated nitric acid, and make up to volume with deionized water.

谢谢啦

那你们按最新CO3的标准是用ICPMS测试吗

原文由 sega741(sega741) 发表:
那你们按最新CO3的标准是用ICPMS测试吗

没，限定值变了吗？不就是Cd是100ppm,其他还是1000ppm

不会吧，五种可迁移都一直是1000啊，

原文由 sega741(sega741) 发表:
不会吧，五种可迁移都一直是1000啊，

不好意思记错了，HASBRO关于涂层这块做C-03对AS的限定值是100ppm,请看附件

原文由 sega741(sega741) 发表:
那你们按最新CO3的标准是用ICPMS测试吗

我们用ICP-OES测

4 Experimental Procedure
4.1 Scrape off the applied coating from the test sample with a scalpel, or other
suitable scraping tool, being careful not to remove any of the underlying
substrate material. Alternatively, the coating can be removed with
tetrahydrofuran (THF) or a suitable solvent (Note 2). Collect into an appropriate
weighting vessel, evaporate the solvent from the removed coating and dry to
constant weight (to the nearest 1 mg) in an air convection oven at 60°C ± 3°C
for at least 1 hour. This may take several hours. Record the drying time in the
oven Log book. Remove the vessel from the oven and cool in a desiccator.
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 a
pestle 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 :m
sieve. 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.
4.3 Transfer a sufficient amount (i.e 5g) of the standard reference material (NIST
1633b or NIST 2710) to an appropriate vessel. Dry it as required by the
certificate of analysis, in an air convection oven at 60°C ± 3°C for at least 1
hour. Remove the vessel from the oven, cool and store in a desiccator.
4.4 Prepare the 5% (v/v) HCl leaching solution by diluting 50 mL of concentrated
(approx. 37% w/w) hydrochloric acid to 1000mL with ultra-pure water.
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.
4.6 Control sample
4.6.1 Transfer about 100 mg of the standard reference material (NIST 1633b
or NIST 2710) 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 wit h the use of digital
shaker (140 speed) 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. Prepare this
control in duplicate.
4.7 Method blanks
4.7.1 Prepare a blank solution by adding 20 mL of the 5% (v/v) HCl leaching
solution to a 100 mL beaker and immediately start stirring for 10 ± 1 min.
at 20ºC ± 3ºC with the use of digital shaker (speed 140) or a magnetic
stirrer. At the end of the 10 ± 1 min. 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.
4.8 Prepare a 2.0% (v/v) nitric acid diluting solution by diluting 20 mL of concentrated
(approx. 69% w/w) nitric acid to 1000mL with ultra-pure water.
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.
这好像是最新版的，2011-8-18