I Have a Research Support System

Back in the office, Xu Qiu received an unexpected message.

"Senior sister will use pyridine in this afternoon's experiment?" Xu Qiu was surprised. He knew that pyridine was a big killer, and its toxicity was the second.

For example, there are many similar questions on the Internet, "What is the experience of taking a breath of pyridine?" "If you are given 10 million, but the price is to smell the smell of pyridine every day, how would you choose?"

"Well... I forgot to mention it before, and I just noticed it when I was preparing for the experiment." Chen Wanqing made an apologetic expression and explained: "The last step of connecting D and A units requires pyridine as a catalyst and chloroform as a solvent. .”

"The last time senior sister synthesized..." Xu Qiu recalled it, and suddenly said: "Oh, I remembered, the last time happened to be on Saturday, and we were not there."

"Yes," Chen Wanqing nodded, and continued: "My suggestion is that you finish the experiment first, and then after I finish using pyridine, we can directly end our experiment today, and the rest of the time can be used to write reviews or paddle What."

"I'm fine. The experiment can be done before evening." Han Jiaying agreed, and it seemed that the two had already discussed it.

"Since this is the case, I'm fine. I just don't have much experiment content today, so let me pass a pillar later." Xu Qiu nodded in agreement. The senior sister's suggestion is very reliable. The laboratory can't work normally all day, unless the experiment is forced with DEBUFF.

"Okay, then I will hand over the laboratory to you two in the afternoon, and I will submit a response in the evening." Chen Wanqing said.

Upon receiving this news suddenly, Xu Qiu went directly to the laboratory without taking much rest.

Although the three of them discussed the experiment plan, there may be uncertain factors in the actual experiment process, and the plan may change at any time. If the experiment between him and the junior is not completed at night, it will drag down the progress of the senior.

Therefore, it is still necessary to make a quick decision.

Xu Qiu put on his lab coat and gloves, turned off the vacuum oven, took out the dried third-generation 3D-PDI crude product from the vacuum oven, dissolved it in dichloromethane again, mixed the sample, and loaded the sample column.

The disposable blank silica gel column has been completely used up, but he did not choose the reusable sample column.

The main reasons are, one is that it is more troublesome to fill in the columns by hand, and now it needs to save time, and the other is that he is also prepared.

Xu Qiu took out the disposable columns used before. On the plastic casing of these old silica gel columns, there were some marks he had made with a marker pen before, which contained the composition of the previously separated and purified samples.

After picking for a while, he picked up a relatively short, clean-looking silicone column.

Because they are all PDI systems, even if some of the deadly adsorbed molecules in the column are eluted with an eluent of similar polarity, there is a high probability that they will not be desorbed again.

Even if a little molecule is desorbed, it will have little effect on the product. For the optoelectronic materials used in the preparation of organic photovoltaic devices, a purity of 99% can already meet the basic needs.

There is no perfect thing in the world, and it is definitely unrealistic to guarantee 100% purity of samples.

Connect the sample column and blank silica gel column to the liquid chromatograph, confirm that there is no problem with the test tube rack, solvent, and waste liquid bucket, and turn on the instrument.

...

This time there was only about 40 mg of crude product, and the polarity difference between several sample points was not big, so the separation and purification were not difficult, and Xu Qiu completed it in just over an hour.

However, because the amount of the product is too small, the product seems to be evenly plated on the inner wall of the bottle during the process of rotary evaporation to dry up the solvent, dark red, with only a thin layer.

'It's a little troublesome. ’ Xu Qiu smashed his mouth, and patiently scraped the product off the eggplant-shaped bottle wall with a stainless steel scraper, just like plowing the ground, where the scraper and the bottle wall contacted, forming a gully.

The scraper and the curved glass bottle wall are almost in point contact. If you want to get as much product as possible, you have to traverse most of the points in the bottle, which is a test of patience.

Ten minutes later, Xu Qiu took down most of the product, collected it in a glass bottle, weighed it, and obtained a total of 33.1 mg of the product.

The yield is not bad, about 80%.

Copy the third-generation 5 series 3D-PDI synthesized this time to Simulation Lab II, and arrange simulation experimenters to explore device performance.

Having successfully completed today's experimental task, Xu Qiu is in a good mood.

He looked around the laboratory, Han Jiaying was processing the reaction in front of the fume hood, and then walked towards her.

Looking at the back of the junior girl in a white coat and operating steadily, it is really difficult to connect with her who is usually lively and jumpy.

When he was approaching Han Jiaying, Xu Qiu deliberately made some noise with his shoes.

This time he didn't want to make a surprise attack, the school girl was still holding the reaction bottle in her hand, if she accidentally frightened the other party and made her shake the product away with a shake of her hand, that would be bad.

"Brother?" Han Jiaying obviously heard the commotion behind her, stopped what she was doing, and tilted her head.

"Well, my experiment is over, I'm here to see you." Xu Qiu explained.

Han Jiaying turned around, continued the experiment, and then briefly stated the results, "I ordered the plate just now, and the yield of the two reactions is estimated to be around 50%. There are quite a lot of by-products, but the polarity difference between them is not small. It shouldn't be difficult."

"No way, the central nuclear unit is relatively large, which may indeed cause a decrease in production rate." Xu Qiu randomly guessed a reason, which was considered comforting.

"Well... By the way, our disposable blank silica gel column is used up, and this time we have to repack the column. Did the brother install the column manually just now?" Han Jiaying asked. Autumn has already started going through the pillars, so not really sure.

"That's not true..." Xu Qiu briefly said what he did just now, and then said: "However, sooner or later, you will have to install the column manually, so I will teach you today, and we will share one of the two products later."

"That's great." Han Jiaying nodded happily, pointing to an oil bath next to her, "Brother, please."

"You're really being rude to me." Xu Qiu smiled, and naturally he didn't refuse, and it didn't take much time to deal with the reaction.

The two reactions of the school girl are the synthesis of the first generation of 3D-PDI, using two nuclear units designed by herself, 3TB and 4TB, and the PDI molecule used is PDI-6, so the names are PDI3-3TB-6, respectively. PDI4-4TB-6.

The type of reaction is the Suzuki reaction. Xu Qiu has done it many times before, so he is familiar with the post-treatment. The product is dropped into methanol solution, vacuum filtered by Buchner funnel, and dried in a vacuum oven.

Then, he took out two bags of silica gel from the cabinet under No. 5 fume hood and transferred them to the fume hood for inorganic synthesis.

The main component of silica gel is amorphous silica, which has stable chemical properties and generally has specifications such as 100-200 mesh, 200-300 mesh, and 300-400 mesh.

Xu Qiu took the box containing the blank silica gel column, turned around and asked, "Sister, what is the approximate quality of the product?"

"Probably..." Han Jiaying thought for a while and said, "About 100 milligrams. It's an exploratory experiment. I didn't dare to feed more. At this point in the reaction, there is only so much left."

"Then there is no need to choose a too thick silica gel column..." Xu Qiu muttered while picking out a silica gel column from the box.

In the end, he picked two relatively short pillars, the same size, about 20 centimeters in length, and about 3 centimeters in inner diameter. He nodded in satisfaction, "Just them."

Han Jiaying took one of the silicone pillars and stood aside obediently.

Xu Qiu took a plastic funnel and a disposable PE cup, unscrewed the upper end of the silica gel column, inserted the funnel, then used the PE cup as a spoon, added 300-400 mesh silica gel to the silica gel column, and introduced:

"The larger the mesh number of silica gel, the smaller the silica gel particles, the best adsorption effect, the smaller the mesh number, the larger the silica gel particles, the poorer the adsorption effect. Previously, 100-200 mesh silica gel was used for mixing samples. Normal blank silica gel The column usually uses 300-400 mesh silica gel."

After it was installed to about 90% of the height of the silica gel column, Xu Qiu stopped adding silica gel, put several layers of toilet paper on the experimental bench, held the silica gel column with both hands, and vertically vibrated it back and forth on the paper surface, making "duang" "duang" ", explaining:

"Although the silica gel is filled now, it is not compact and uneven. The silica gel needs to be solidified. Otherwise, after the solvent is introduced later, the column may break, or the sample may pass through the side of the column quickly. "

"It's like... a side leak?" Han Jiaying tilted her head.

"What are you thinking, every day." Xu Qiu was speechless for a while, then thought carefully, and said, "However, the metaphor is quite appropriate."

Xu Qiu "duang" for about a minute. Seeing that the height of the silica gel column had dropped a lot, he stopped, and added some more silica gel to it to make it up to about 90% of the height, and continued to vibrate up and down.

Afterwards, Han Jiaying followed suit and began to fill in the pillars, and began to dance the silicone pillars up and down, like a low-powered pile driver, "Brother, how long will it take to do this?"

"Until the height of the silica gel column no longer changes with the vibration," Xu Qiu paused and said, "To be conservative, fifteen minutes."

Later, he explained: "There is no quantitative standard for this. Only when the column is formally used will the effect be known. The main reason is that the consequences are serious. If the column is broken, the product must be washed down with a highly polar solvent. , reload the post, and do it all over again, so try to get it right.

In fact, it was easier for us to do the column experiment before. The disposable blank silica gel column that does not need to be manually filled has played a great role, significantly reducing the failure rate of the experiment. "

"I understand." Han Jiaying nodded.

After more than ten minutes, Xu Qiu let out a long breath, stopped what he was doing, and said, "It's almost finished."

"I'm getting better soon, but... my hands are a little sore." Han Jiaying's current state was like a pile driver with insufficient power.

"Well, but the sample is still drying, and I can't take it out for a while, so I can't put it in." Xu Qiu turned his gaze to the vacuum oven, just in time to see a batch of waste liquid buckets next to him, and suggested:

"Why don't you take advantage of this gap to dispose of the waste liquid?"

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