| Pages:
1
2 |
PHILOU Zrealone
International Hazard
Posts: 2893
Registered: 20-5-2002
Location: Brussel
Member Is Offline
Mood: Bis-diazo-dinitro-hydroquinonic
|
|
Hi Sauron,
Maybe the following procedure will work with less troubles:
1°)Fit the page in the Google Book link with the zoom tool to get the full page at screen.
2°)Alt-Ctrl-Print Screen
3°)In an open word document Ctrl V adjust the margins to minimal in a way to maximise image into the word document.
4°)Save with name x.doc
5°)Do a pdf of x.doc to make a x.pdf document.
6°)With the selection tool make a selection window into your x.pdf to fit the book page at best.
7°)In an open word document Ctrl V adjust the margins to minimal in a way to maximise image into the word document.
8°)Save with name final.doc
9°)Do the same procedure from 1°) to 6°) but for page 2
10°)Open final.doc go to the end of the page after the last image eventually set a page break ina way to be certain the next image
goes to the next page then Ctrl V adjust the image in a way to maximise image into the word document.
11°)Save with name final.doc
12°)Repeat procedure from 9°) to 11°) for next pages.
13°)When the document is large enough and that you have all wished pages
Do a pdf of final.doc to make a final.pdf document.
In the word programma you can eventually make a landscape to put 2 images next to each other per page...making the final document look like the
original book and maybe improving the scan quality by zooming a bit out.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
|
|
|
Sauron
International Hazard
Posts: 5351
Registered: 22-12-2006
Location: Barad-Dur, Mordor
Member Is Offline
Mood: metastable
|
|
Won't that screen dump give me everything and not just the page window?
And at screen resolution?
Thanks for suggestion anyway.
Sic gorgeamus a los subjectatus nunc.
|
|
|
not_important
International Hazard
Posts: 3873
Registered: 21-7-2006
Member Is Offline
Mood: No Mood
|
|
In this case the OCRed version seemed quite good, I wonder if Google has enhanced it recently. The only serious problem was around numbers with
decimals, 0:O, 1:l or I, and 5:S being the most common. That's what I corrected, the rest of the text save one equation looked good.
Your image capture looks to be Windows & IE specific. For Firefox the Web Developer plug-in will show all images, which in this case includes the
current, previous, and next pages as PNG images. Save the images, giving them unique names, then page forward 3 pages to get the next triplet. I did
that to start with, but the text view looked so good that I went that route.
|
|
|
Sauron
International Hazard
Posts: 5351
Registered: 22-12-2006
Location: Barad-Dur, Mordor
Member Is Offline
Mood: metastable
|
|
Yes it is IE specific. The webpage with instructions specifically mentioned it would not work for Firefox.I regard it as an emergncy expedient
procedure only.
Now that it is clear that Gladstone was talking about mercury (I) chloride, calomel, and not the bichloride, the stoichiometry is shown to be
PBr3 + 3 HgCl -> PCl3 + 3 HgBr
Yeah I know HgCl is really Hg2Cl2 and likewise for the bromide, but equations with noninteger components make me uneasy.
Bottom like is MW PBr3 is 267, and that of Hg2Cl2 is 478. So it takes c.700 g Hg2Cl2 to change 1 mol PBr2 to PCl3. In that process, the phosphorus
compound loses 132 g/mol while the Hg compound gains same.
We are left after distillation with 830 g Hg2Cl2 in the pot and 130 g PCl3 in the receiver.
The problem therefore is recovering the Hg2Cl2 as such because the bromide is no good to us.
It is insoluble in water, as it is non-ionic. I would like to find a direct transformation to Hg2Cl2 but I fear that it is more likely that it will
have to be recovered as Hg metal, dissolved in cold dilute HNO3 then precipitated with NaCl.
Any shortcut to Hg2Cl2 from mercurous bromide?
[Edited on 20-2-2009 by Sauron]
Sic gorgeamus a los subjectatus nunc.
|
|
|
Sauron
International Hazard
Posts: 5351
Registered: 22-12-2006
Location: Barad-Dur, Mordor
Member Is Offline
Mood: metastable
|
|
I spent last night and this morning trying the usual sources for information on Gg2Cl2 prep beyong what I have above.
Inorg,Syn, nothing
Brauer, nothing
Merck, no references
Ullmann, one reference but AFAIK inaccesible:
Pharm. Ztg. (1930) p 11
The 1911 Britannica is a bit more helpful. Solutions of stannous chloride will reduce Hg2Br2 to Hg2Cl2, and if in excess, to Hg metal. So I can
recycle the Hg2Cl2, and when done preparing PCl3, recover the Hg metal.
I would still like to have a little more quantitative information, such as the best molar concentration of HNO3 for dissolving Hg ("cold dilute")
being a little vague) the rest can be worked out via stoichiometry. The mercurous nitrate soln in dil HNO3 is used in situ to react with NaCl, the
precipitate being very dense will settle fast, supernate decanted and the powder washed free of acid then dried with absolute ethanol to remove water,
then vacuum dessicated. Then it is ready for PBr3,
Sic gorgeamus a los subjectatus nunc.
|
|
|
not_important
International Hazard
Posts: 3873
Registered: 21-7-2006
Member Is Offline
Mood: No Mood
|
|
| Quote: | 5. Mercurous Nitrate or Nitrate of Suboxide of Mercury,
Preparation.—1 part of pure nitric acid of 1.2 sp. gr. is poured on to 1 part of pure mercury in a porcelain dish, and the vessel allowed to remain
for twenty-four hours in a cool place; the crystals which are formed are separated from the undissolved mercury and the mother liquor, and dissolved
by grinding them up in a mortar with water which has been previously mixed with one-sixteenth part of nitric acid. The solution is filtered and kept
in a bottle with some metallic mercury sufficient to cover the bottom of the vessel.
Tests.—With dilute hydrochloric acid, the solution of mercurous nitrate should give a copious white precipitate of mercurous chloride; sulphuretted
hydrogen should produce no precipitate in the filtrate from this, or at most only a trifling black precipitate (sulphide of mercury).
|
Qualitative Chemical Analysis By C. Remigius Fresenius, Charles Edward Groves 1887
Queen Victoria is a friend of the chymist.
|
|
|
Sauron
International Hazard
Posts: 5351
Registered: 22-12-2006
Location: Barad-Dur, Mordor
Member Is Offline
Mood: metastable
|
|
Thanks. There is also a prep in "Synthetic Inorganic Chemistry" in the forum library, employing 25 g Hg and 20 ml 6 M HNO3, again a slight excess of
acid. This is a 125 mmol scale.
So one would then add an equivalent of NaCl as a satd soln I suppose and Hg2Cl2 will drop out..
I have at least a Kg Hg on hand, this beats the hell out of paying Acros an absurd price for Hg2Cl2. They want $400 US/Kg, almost and by the time it
gets here I will be paying $750 US.
Whew! glad to dodge that bullet.
Thanks once again!
By the way, folks, this procedure releases a lot of NOx, so trap it and scrub it or do it in the hood.
Here is the German version of Gladstone's article, this in J.prakt.Chem.
I will have to wade through this to see if Dr.G. said anything about Cl2 displacing Br on PBr3 as attributed by Mellor.
[Edited on 20-2-2009 by Sauron]
Attachment: JPraktChem,1850,49, pp40.pdf (562kB)
This file has been downloaded 716 times
Sic gorgeamus a los subjectatus nunc.
|
|
|
Sauron
International Hazard
Posts: 5351
Registered: 22-12-2006
Location: Barad-Dur, Mordor
Member Is Offline
Mood: metastable
|
|
Gladstone does say that the relative affinity for P of the halogens is Cl>Br>I and yes he does specifically state that this exchange is
accomplished by either the elemental halogen or, by the Hg(I) halide.
Thus, per Gladstone, PI3 is converted to PBr3 by Br2 or, by Hg2Br2. PBr3 is converted to PCl3 by Cl2 or Hg2Cl2. I2 has no such effect on either PCl3
nor PBr3 and neither does Hg2I2.
PI3 is too costly to be of use in this fashion of course.
The bone I have to pick with MEllor is that Gladstone was specifically talking about mercurous halides but Mellor cited Gladstone as saying this
reaction is performed by mercuric halides. Gladstone did not claim this. We now have Gladstone in black and white in English and German and nowhere
does he say mercuric chloride HgCl2, or bichloride of mercury, or corrosive sublimate. He gives the equation and it is for HgCl (corresponding to
Hg2Cl2) and he names it as chloride of mercury not bichloride.
Now for all I know HgCl2 may work, but the point is that, that isn't what Gladstone wrote.
So it always pays to go to sources.
[Edited on 21-2-2009 by Sauron]
Attachment: Page 1033 from Mellor ACTOITC 8 N_P.pdf (112kB)
This file has been downloaded 567 times
Sic gorgeamus a los subjectatus nunc.
|
|
|
Sauron
International Hazard
Posts: 5351
Registered: 22-12-2006
Location: Barad-Dur, Mordor
Member Is Offline
Mood: metastable
|
|
I just downloaded the classic 63 page Baudrimont paper from Ann.Chim.Phys. (1864) so frequently cited in Mellor Vol VIII, on the chlorides and
bromides of phosphorus.
[Edited on 21-2-2009 by Sauron]
Attachment: Baudrimont.pdf (2.1MB)
This file has been downloaded 491 times
Sic gorgeamus a los subjectatus nunc.
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
