Determination of Paraffin Wax Content

Standard: BS EN 12606-1:2015

Procedure
1. Pour each test portion 25 ± 1 grams each into the distillation flask and weigh to
the nearest 10 mg (mass mB). Heat the distillation flask in the burner such that the
first distillate drop falls down after 3 minutes to 4 minutes.
2. The vapors produced during distillation are condensed in an Erlenmeyer flask
immersed in a mixture of finely ground ice and water. Adjust the distillation rate
such that 15 ± 5 drops fall from the end of the outlet tube every 10 seconds.
3. Complete the distillation in 14 minutes and a maximum of 15 minutes. Mix the
distillate by gently warming and swirling the receiver.
4. Cool the receiver to ambient temperature and weigh the distillate contained in the
receiver to nearest 10 mg (mass mD). Add 2-4 grams (3 gram is recommended) of
the distillate into the test tube and weigh to the nearest 5 mg (mass mE).
5. Dissolve the weighed mass of distillate in 25 ± 1 ml of ether and add 25 ± 1 ml of
ethanol. Close the test tube and place it in a cooling bath maintained at -22 ± 10C
6. Transfer 20 ± 1 ml of washing liquid into the test tube fitted with wash bottle head
and cool in the cooling bath to -20.0 ± 0.50C.
7. Place the round filter in the funnel in the cooling bath and connect it to filter flask.
Quickly transfer the slurry of crystals produced at -20.0 ± 0.5 0C to the filter. Rinse
the test tube with the cooled washing liquid. Distribute washing liquid as
uniformly as possible between three washing operations.
8. Support the filtration by gentle vacuum process during which pressure does not
fall below 5 kPa. Lift the round filter using pincers, place it in evaporating basin.
Dissolve crude paraffin wax residue by carefully spraying petroleum spirit over it.
Dissolve any paraffin wax in the test tube or temperature transducer.
9. Evaporate the mixed filtrates in the evaporating basin. Dry the residue for 15 ± 1
minute at 125 ± 50C in the oven and allow it to cool.
10. When waxes have cooled down and have not quite solidified, add 15 ml of
acetone. Dissolve the paraffin wax by gently heating and carefully swirling the
evaporating basin.
11. Cool the acetone-paraffin wax solution in a water bath to 15.0 ± 0.5 0C. Separate
by filtering the paraffin waxes that filter out.
12. Wash the evaporating basin, temperature transducer and filter several times with
acetone brought to 15.0 ± 0.50C from a wash bottle ensuring that the total volume
of wash liquid is 30 ± 1 ml. The washing liquid shall be discarded.
13. Dissolve the purified paraffin wax by spraying them with heated petroleum spirit
 and collect them in the same evaporating basin. Evaporate the petroleum-paraffin
wax solution in a weak air stream over the water bath.
14. Dry the crystallized paraffin wax for 15 ± 1 minute at 125 ± 5 0C in the oven and
allow it to cool. Determine the mass to the nearest 0.5 mg (mass mA).
15. If the final mass is outside the range 65mg to 85 mg, reject the result and repeat
the test with adjusted initial mass of the same distillate (mass mE).
16. If the initial mass which is required to give final mass between 65mg and 85mg, is
below 2g or above 4g, record this in the test report.

石蜡含量的测定
标准：BS EN 12606-1：2015

程序
1.将每个测试部分各 25±1 克倒入蒸馏瓶中，并称重至最接近的 10 毫克（质量
mB）。在燃烧器中加热蒸馏瓶，使 3 分钟到 4 分钟后第一滴馏出液掉落。
2.蒸馏过程中产生的蒸气在锥形烧瓶中冷凝，该锥形烧瓶浸在细碎的冰和水的
混合物中。调整蒸馏速率，使每 10 秒从出口管的末端掉落 15±5 滴。
3.在 14 分钟内完成蒸馏，最多 15 分钟。通过轻轻加热并旋转接收器来混合馏出
液。
4.将接收器冷却至环境温度，并将接收器中包含的馏出物称重至最接近的 10
mg（质量 mD）。将 2-4 克（建议 3 克）馏出物加到试管中，称重至最接近的 5
毫克（质量 mE）。
5.将称量的馏出物溶解在 25±1 ml 的乙醚中，然后添加 25±1 ml 的乙醇。关闭试
管，将其放入保持在-22±10C 的冷却浴中
6.将 20±1 ml 洗涤液转移到装有洗涤瓶盖的试管中，并在冷却浴中冷却至 -
20.0±0.50C。
7. 将 圆 形 过 滤 器 放 入 冷 却 浴 的 漏 斗 中 ， 然 后 将 其 连 接 至 过 滤 瓶 。 快 速 将 -
20.0±0.50C 产生的晶体浆液转移到过滤器中。用冷却的清洗液冲洗试管。在三
个洗涤操作之间，应尽可能均匀地分配洗涤液。
8.通过温和的真空过程支持过滤，在此过程中压力不低于 5 kPa。用钳子提起圆
形过滤器，将其放入蒸发池中。通过在其上小心喷洒石油溶剂溶解粗石蜡残渣。
将所有石蜡溶解在试管或温度传感器中。
9.在蒸发池中蒸发混合的滤液。将残留物在烤箱中于 125±50°C 下干燥 15±1 分
钟，然后冷却。
10.蜡冷却下来并没有完全固化时，加入 15 毫升丙酮。轻轻加热并小心旋动蒸
发盆，以溶解石蜡。
11.在水浴中将丙酮-石蜡蜡溶液冷却至 15.0±0.50C。通过过滤分离出的石蜡进行
分离。
12.用从洗瓶中升至 15.0±0.50C 的丙酮清洗蒸发池，温度传感器并过滤几次，确
保洗液总量为 30±1 ml。清洗液应丢弃。
13.通过用加热的石油精喷洒溶解的纯石蜡，并将它们收集在同一蒸发池中。在
水浴上方的弱气流中蒸发石油-石蜡溶液。
14.将结晶的石蜡在烤箱中于 125±50°C 下干燥 15±1 分钟，然后冷却。确定质量
至最接近的 0.5 mg（质量 mA）。
15.如果最终质量不在 65mg 至 85mg 范围内，则拒绝该结果，并使用相同馏出物
（质量 mE）的调整后初始质量重复测试。
16.如果要使最终质量介于 65mg 和 85mg 之间所需的初始质量小于 2g 或大于
4g，则将此记录在测试报告中。