#FILE .discard # Last edited on 2019-10-20 01:38:32 by jstolfi GALLEY TRANSCRIPT OF LAB NOTEBOOKS This text should be moved to the notebooks of individual experiments. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-21-Tue-s1.txt ammonium phosphate fertilizer Solubility of NH4.H2PO4 (ADP; molar mass 115.02) in H2O (molar mass 18.015): temp g/100ml x -5 22.6 0.184 0 24.9 0.199 5 27.5 0.216 10 30.3 0.233 15 33.4 0.250 20 36.8 0.269 25 40.6 0.289 30 44.7 0.309 35 49.3 0.330 40 54.3 0.352 45 59.9 0.375 50 66.0 0.398 55 72.7 0.421 60 80.2 0.445 65 88.4 0.469 70 97.4 0.493 75 107.4 0.518 80 118.4 0.542 85 130.4 0.566 90 143.8 0.590 95 158.5 0.613 100 174.7 0.636 105 192.5 0.658 Not clear whether this experiment was carried out or only planned: Dissolved 94 g of crystallized ADP in 117 g H2O at 60 C forming a saturated solution. On cooling to 38 C, 54 g crystallized (A14); saturation should be 52.3 g/dL. On cooling to 34 C, 25 g crystallized (A16); saturation should be 48.3 g/dL. On cooling at 29 C, 15 g crystallized (A18); saturation should be 43.9 g/dL. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-07-Dom-s1.txt cobalt_pigment Trying to dissolve the cobalt pigment by first treating with concentrated NaOH. Placed 1 g of pigment and 2 g of NaOH flakes in a beaker (previously frosted by NaOH) with enough water to dissolve the latter. The suspension was dark lilac almost purple. Heated in BM for 10-20 minutes. Color became darker and grayer; a gray-black film formed on top. Final color was blue-black. Not much change was visible in microscope. Diluted with water and filtered through 28 um paper. Filtrate (MC1) was light purplish blue, cloudy. Dilution made the ppt (MC4) lighter a bit: purplish gray. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-12-28-Thu-s1.txt cobalt_pigment Got a modest amount of "cobalt coloring" for ceramics, a very fine light lavender powder. Label says "VDM F202" but Google can't find that code. The colorant seems to be a frit. Microscope examination shows irregular grains, like glass fragments. Some are clear, mostly colorless or very light yellow, orange or pink. Others are intense blue, nearly black; only the smallest ones look transparent. Trying to extract the cobalt by acids. In each of two 10 mL beakers, put 1 g of coloring. In one beaker (MC2) put 1-2 mL of acetic acid glacial plus some water qsp 4 mL. In the other beaker (MC3) put 1-2 ml of lactic acid 85% plus some water qsp 4 mL. There was no immediate reaction. After 3 days Beaker with acetic acid (MC2) had 2 mm of lilac ppt and 3 mm of a rose-purplish clear liquid on top. Microsc. the ppt is qualitatively similar to the untreated coloring. Beaker with lactic acid (MC3) had 5 mm of dense pink ppt and only a litle light pink liquid on top. Microsc. the ppt showed qualitatively simlar to original pigment but mixed with many slightly yellow or pink clear crystals, with rectangular appearance, sharply-cut ends, about 5-10 times longer than wide. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-12-28-Thu-s1.txt lead melting Melted some lead fishing weights of two shapes (round and elliptical) on the large electric stove. Reached easily the fusion temp (327 C) and higher by wrapping aluminum foil loosely around an inox drinking cup. Pyrometer showed ~340 C just before pouring. Poured on a conical inox flask in a covered holder made of cement. Added more weights and repeated. After cooling, scraped the wider base with a sharp flat wood chisel to make it flatter. Saved the shavings in a bottle (L1). Larger ingot (1) is 302 g weight, 39.6 mm high, with base diameters of 24 mm and 35 mm. Computed volume is 27.4 mL. Computed density is 11.0 g/mL, very close to pure lead's 11.34 g/mL. Smaller ingot (2) is 272 g weight, 36.8 mm high. Computed diameter of larger base is 34 mm. Computed volume is 24.5 mL. Computed density is 11.1 g/mL. Some slag and metal adhered to the inox crucible, and only some of it could be removed. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-02-Tue-s1.txt yam_anthocyanin Discarded (Z1) (Z2) (Z3) (1h) (2h) (3h) (4h) because they were too moldy and disgusting. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-09-24-Dom-sX.txt yam_anthocyanin (Date approximate) Filtered some of the fermented purple yam juice. Used my epoxy-sealed kitasato and conical funnel with aquarium pump. Left the filtrate (Z0) in the kitasato (~100 mL). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-10-01-Dom-s1.txt yam_anthocyanin Filtered the starch from the last run. Used the ground-glass kitasato+buchner with 28 um filter paper and aquarium pump. Was fast and left the starch quite dry. Today there was a layer of mold on the filtrate (Z0). White, fluffy, with dark gray-black fruiting bodies sticking up, about 1 mm tall and a fraction mm diameter. Took a mutifocus stack of pictures with the Eagle microscope and with the Celestron camera on the Vostro laptop. Transferred the rest of the fermented and moldy yam juice (~600 mL) to a beaker, removing the white mold layer on top. Added 2 tsp ofcitric acid (Z1). Consistency like thick soup, brownish red, rotten yam smell. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-12-11-Mon-s1.txt yam_anthocyanin Tried to filter (Z1) with vacuum on ground-glass kitasato+buchner and aquarium pump. Clogged filter after a few drops of light brownish filtrate (Z3). Returned unfiltered part to beaker. Added to (Z1) 5 g of Al2(SO4)3 dissolved in water and filtrated to remove cloudiness. Result (Z2) is brown paste. Tried to filter again. Clogged again after a few drops of clear colorless filtrate, added to (Z3). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-14-Dom-s1.txt cobalt coloring Filtered (MC3) with water washing yielding (MC13) nearly colorless liquid and (MC14) pink paste. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-12-Fri-s2.txt Two small samples of ppt (MC8), about 4 mm diam and 0.5 mm thick, were placed in test tubes. To sample (MC8a) added ~1.5 mL ofacetic acid glacial. Slowly developed pinkish hue, but the flakes of the (MC8) ppt did not even disperse. To sample (MC8b) added ~1.5 mL of lactic acid 85%. Vigorous bubbling. Flakes of (MC8) disintegrated. Slight pink color developed and liquid became cloudy. Heating the suspension (MC7) to boiling. Fine black ppt in suspension. Filtered with 28 um paper, yielding (MC9) clear blue liquid and (MC10) black powder ppt. Filtered (MC2) with water washing yielding (MC11) pink clear liquid and (MC12) lilac ppt. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-13-Sat-s1.txt On drying the filter paper with the (MC10) ppt on a hot plate, a canary yellow halo appeared where the liquid had diffused and dried out. The greenish-black ppt adhered to the paper like a layer of paint and was impossible to scrape off. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-04-30-Sun-s1.txt Checking the NAOH from Loja Quimica. Placed 30.74 g on a "stainless" steel cup (tare 44.48 g). Heated on electric stove. Melted with little bubbling. At over 140 C (off therm. scale), a "rust" came off the can, turning the mass brick-colored (S1). Weight after cooling: 29.20 g (lost 1.54 g). Poured into beaker, washed can with a little H2O. On cooling solidified into light brick orange mass, hard and adhering to the beaker. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-05-01-Mon-s2.txt Checking the NAOH from Loja Quimica. The top of the solid (S1) absorbed water from air creating a thin liquid layer with a light brick orange suspended ppt. Heated the beaker again; boiled at over 145 C (off therm scale). Placed drop of (S1) on aluminum foil (S3). ------ In erlen (tare 75.67 g) placed 10.00 g NaOH.(H2O)x, flakes, and 15 g of water at 33 C. Temperature rose to 75 C in spite of cold erlen. Reweighted when boiling at 118 C: 22.84 g (lost 2.16 g). Boiled some more, forgot to note temp. Weight 21.90 g (lost 3.10 g?). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-05-16-Ter-s1.txt solubility of NaOH Checking the boiling point of NaOH solutions. Placed in an erlen (52.31 g tare) 5 g NaOH(H2O)x, flakes, and 10.4 g H2O. Re-weighted when boiling at 112 C: 12.23 g. Added H2O to 15.20 g. Re-weighted when boiling at 120 C: 11.79 g. Re-weighted when boiling at 130 C: 9.47 g. Poured off on metal dish (T1) ------ Discarded (S1) minus sodium aluminate(?) crust (S4). Dissorved (S4) in hot water. Poured some (T1) on aluminum foil. Kept adding while bubbling. Added (S4) too. ---------------------------------------------------------------------- unknown date sodium phosphates NaH2PO4 d 2.36 g/mL sol 59.9 g/dL Na2HPO4 hydrates 2, 7, 8, 12 pH 8-11 d 1.7 g/mL MP 250 C dec sol heptahydrate 7.7 g/dL at 20 C sol heptahydrate 18.8 g/dL at 25 C insol ethanol Na3PO4 orthorombic used for cleaning pH 1%: 12 dissolves copper oxide at high temperature MP 1583 C d anhydrous 2.536 g/mL insol ether sol water anydrous g/dL: 0 C 5.4 20 C 12 25 C 14.5 40 C 23.3 100 C 94.6 dodecahydrate: MP 73.4 C BP 100 C ---------------------------------------------------------------------- unknown date ammonium phosphates NH4H2PO4 sol ether d 1.80 g/mL MP 180 C sol water 40.4 g/dL at 25C (NH4)2HPO4 starts decomp emitting NH3 at 70 C avg pH 7.5-8 insol ether sol water g/dL: 10 C 57.5 100 C 106.7 MP 155 (decomp) d 1.619 g/mL (NH3)3PO4 unstable, no commercial value. ---------------------------------------------------------------------- Solubility data of NH4H2PO4 from various sources. Some may be hydrated? Date: 1920 mass fractions 0 C 0.300 10 C 0.384 20 C 0.408 30 C 0.425 40 C 0.450 50 C 0.470 60 C 0.494 70 C 0.514 Date: 1936 mass fractions 192 C 0.832 182 C 0.820 161 C 0.730 126 C 0.649 120 C 0.622 Date: 1947 mass fractions 0.0 C 0.304 4.0 C 0.320 8.4 C 0.340 10.6 C 0.352 12.2 C 0.360 15.8 C 0.384 16.5 C 0.390 26.0 C 0.404 Date: 1967 mass fraction -4.5 C 0.180 (?) -4.0 C 0.170 -2.0 C 0.100 (?) -1.6 C 0.190 +2.5 C 0.200 +9.5 C 0.225 +22.5 C 0.275 +32.5 C 0.325 +35.5 C 0.340 +39.0 C 0.350 +46.5 C 0.375 +51.5 C 0.400 Date: 1973 mass fraction -4.3 C 0.169 (eutectic) Date: 1911 mass fraction 0 C 0.198 25 C 0.300 25 C 0.290 (?) 50 C 0.410 70 C 0.492 83 C 0.566 ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-10-Fri-s1.txt yam anthocyanin batch 4 Purchased 6 yams at supermarket; weights 170 176 141 171 241 172 g = 1071 g. Washed lightly, scrubbed with dishwashing sponge. Peeled with potato peeler. Peels are 119 g wet. Peeled yam weights 151 157 128 159 224 160 g = 981 g total (so 90 g peels dry). Divided into 4 batches of 252g wet. covered with Majipak adn left in fridge for a few minutes. Lot (1): Placed yam pieces in blender with 300 mL water from filter at 14 C. Ground for 2 min; final temp 27 C (ambient: 28 C). Blended for 30 sec more. Strained through 2 ply of cotton cloth and wringed as much liquid as possible. * Solids 82 g moist (M1), brownish-purplish light pink. * Liquid (M2) 608 g including erlen E5 (~380 mL). Put (M1) and (M2) in fridge at 01:39. Took out (M2) at 02:28. Lot (2): Put yam pieces in blender with 300 mL of (M2). Blended for 2 min. Final temp 24 C. Strained and wringed. Solids (M3) 79 g moist. Merged with (M1). Liquid (M4) 416 g, ~390 mL. Merged with rest of (M2); ~500 mL total. Put solids and liquids in fridge at 02:45. Tokk out at 03:20. Lot (3): Put yam pieces in blender with 300 mL of (M2)+(M4). Blended for 2 min. strained, wringed. Temp solids ~24 C. * Solids (M5) 92 g; brownish purplish pink, somewhat darker than (M1) and (M3). Merged with (M1) and (M3). * Liquid (M6) 405 g ~380 mL (spilled a few mL). Merged with (M2) and (M4) (~600 mL). Put in fridgre at 03:30, took out at 03:50. Lot (4): Put yam pieces in blender with 300 mL of (M2)+(M4)+(M6). (Spilled some 20 mL, recovered ~15 mL dirty, put aside as (MX).) Blended for 2 min high speed. Strained an wringed. * Solids (M7) 106 g moist; merged with (M1)+(M3)+(M5). * Liquid (M8) 390 g; merged with (M2)+(M4)+(M6). ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-10-Xxx-s3.txt Put liquids back in fridge at 04:15. Rewashing solids: Put (M1)+(M3)+(M5)+(M7) in blender with 1000 mL cold filter water. Blended for 2 min, strained, wringed: * Liquid (M10) 909 g light purple opaque, deposits startch. * Solid (M9) light purplish pink-gray, only a bit lighter than previous residues. (Spilled ~1 g.) Wt 330 g -- retained more water than before? Peels: 118 g. Added 150 mL cold H2O, blended for several min. Strained and wringed: * Solids (M11) brownish (more than pink) with yellow tinge. Discarded. * Liquid (M12) purplish brown. Decanted (M10): * Liquid: 872 g, purple, milky. * Solids: white, starchy, dirty with purple stuff. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-11-Sat-s1.txt anthocyanin Decanted (M2)+(M4)+(M6)+(M8) = (M2-8): * Liquid (M2-8a): put in an ~1 L plastic container, put in freezer. * Solids (M2-8b): starchy ppt. Added 250 mL cold H2O, resuspended (M2-8c), put in fridge. Decanted from (M2-8c) the uberliq, ~210 mL, wine colored, slightly cloudy. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-15-Mon-s2.txt cobalt pigment In another test tube (MC18e) added a flake of (MC18) (olive-black ppt), ~5 mm dia, ~1 mm thk, with ~20 mm H2O, and a generous amount of ascorbic acid. Suspension turned from greenish brown milky to reddish brown milky. Dropped H2O2 on the filter paper with residues of (MC14), but nothing happened -- not even H2O2 decompn. Added some ascorbic acid to (MC9) itself. Restored the clear blue color and removed the black cloudiness. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-18-Qui-s1.txt anthocyanin from yam Processed 3 batches of 240 g of purple yam. Added to each batch 200 mL H2O at 13 C, blended for ~5 min at high speed, washed blender with ~50 mL water. Strained through cloth, pressed had. * Solid (AB01): moist gray-purplish residue, 115+90+105 g. * Liquid (AB02): 950 mL dark wine color liquid. Put in shallow pan. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-18-Qui-s2.txt anthocyanin from yam. Ambient temp 32 C. Blended again (AB02) with 500 mL H2O for ~5 min, yielding grey-purplish paste. Strained, wringed: * Liquid (AB05) milky purple * Solid (AB06) grayish purplish moist, 225 g. Decanted (AB01) after several minutes: * Liquid (AB04), 950 mL, dark wine. Did not deposit signif starch after 5 min. * Solid (AB03) pink starch layer ~2mm thk at bottom of 150 x 300 mm tray. Left (AB05) stand in pan for 5 min, then decanted: * Solid (AB07) starch, ~1mm tkh, 120 mm dia. * Liquid (AB08) whitish wine 510 mL. Tried to filter (AB08) with coffee filter. Clogged right away. Filtrate was milky. Mibex (AB06) with enough water to make a lilac thick soup liquid. Heated on stove, then on BM. Turned into a purplish gray brown translucent puree. Taste and smell were unpleasant at first but disappeared after 20 min. After 20 min, diivided in 2 parts. * To one part added 2 tablespoons of sugar plus a bit of lemon and vanilla flavor. Strained through sieve and cooked in BM for ~5 min. After cooling in fridge became firm like pudding, and made a passable dessert. * To the other part added 2 cubes Korr beef stock + Syrian pepper. Cooked in BM for ~5 min. After cooling in fridge became firm like pudding. Tried to use as side dish, but was too salty and the beek flavor was too strong. In the end discarde most of it. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-15-Mon-s1.txt cobalt pigment Concentrated (MC9) by boiling. After ~24 h (MC17) was a bluish black opaque suspension with an off-white ppt at the bottom. Filtered again (MC17) throughg 28 µm paper. * Liquid (MC19) clear very light blue. * Solid (MC20) black or dark ppt. Shaking (MC9) apparently increases the black suspended ppt. Perhaps oxidation is the key? Put ~3 mm of (MC9) in a test tube. Added 1.5 mL lactic acid 85%, 1.0 mL H2O. Bubbling. Blue color disappeared, white fluffy ppt formed. In a test tube (MC9d) added ~1cm (MC9) then ~2mL H2O2 30%. The H2O2 decomposed violently in contact with solution. However, by stirring after each drop, the entire liquid was discolored and cloudy, with a suspended black ppt. Then added a little ascorbic acid, not enough to neutralize the NaOH. Solution became clear blue again with no trace of black ppt. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-13-Sat-s3.txt cobalt pigment Noticed that (MC8) developed som e needle-like crystals on its surface; possibly Na2CO3? It was drier and more friable, presumably because of the loss of NaOH. Weight 2.3 g. Added 5.2 g of NaOH flakes in an inox can. Heated on electric stove for 0 min at 327 C. Result was a viscous molten black mass (MC15). Let it cool then added some water. Heated it again to cmplete dissolution minus a few grains. Result was a blue-black liquid (MC16). Filtered (MC16) with 28 µm paper: * Liquid (MC17) clear royal blue. * Solid (MC18) olive black ppt. The inox cup was partly corroded with brown "rust". (MC9) Turned blacker and more opaque with time. Reheating to boiling point restored transpacency and color almost completely. (MC17) turned blackish even before the filtering was over. Precipitate (MC14) was pressed between napkins. Some were contaminated with NaOH that left blue stains on ppt. Microsc. still showed mostly the rod-shaped crystals, slightly pink or yellow. (MC18) was brown after washing. Perhaps contamination from inox cup? Microsc. showed mixture of fine dark particles (navy blue or black) and larger yellow-brown flakes. (MC17) After ~1 h became cloudy with ppt of unclear color. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-01-18-Qui-s3.txt Anthocyanin from yams After several hours decanted (AB04): * Liquid (AB09) very dark opaque clear wine. * Solid starch, 1 mm x 150 mm dia. Merged with (AB03). Heated (AB09) in a pan boiling for ~10 min until smell of raw juice mostly disappeared. Boiled it down to ~670 mL. Added water again to 1000 mL. Added 1 teasp. sugar and 1 packet Fleischmann's yeast. (around 2018-01-19 05:00). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-26-Sun-s2.txt dimy_grass At 60 C, (A48) became a mush of crystals. Added 27 g H2O. Temp dropped to 54 C. Reheated to 60 C to dissolve all. On cooling saturated again at 57 C, crystallized at 55 C. Added more water to total wt 135 g. Dissolved all at 38 C. Decanted at 29.5 C: * Solid (A50) needle-like crystals, tangled, 23.4 g. * Liquid (A51) very light yellow clear, 150 g. Merged with (A29) into (A19). Put (A29) in cooling bath when it was 26 C. Started to crystallize at 7.5 C, more at 7,4 C. Decanted: * Liquid (A52) clear light yellow, 352 g. * Solid (A53) fine crystals, 9 g. Tried to wash with ethanol 92% but collapsed and continued wet. In test tube (E6) placed 4 mL of (A47)+(A45) and 8 mL ethanol 46%. Became slightly cloudy. By 2017-03-01 had deposited a light fluffy white ppt. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-27-Mon-s1.txt Dimy grass fertilizer - ammonium phosphate? Put (A45)+(A47) = (A58), 300 g, in a 400 mL beaker with foam jacket, in an ice bath. Started crystallizing between 25 and 21 C. Washed (A53) (maybe deliquescing) with ethanol 92% (50 mL). Dissolved completely. Filtered with 28 µm paper: * Liquid (A54) 38 g, clear. * Solid (A55) practically nothing, discarded. Tried to decant (A58) at 20 C. Failed: too many small ccrystals, liquid would not come out. Reheated to 28 C. Using 38 g (A54) to dissove/wash (A50) (72 g with beaker). Not evident if dissolved anything. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-27-Mon-s2.txt Dimy grass fertilizer - ammonium phosphate? Heating (A50)+(A54) with double majipak and rubber band in BM. Decanted at ~50 C. * Liquid (??) * Solid (A50) 61 g (wet, with beaker). Added 11 g ethanol 99%. Decanted at ~36 C: * Liquid (A57) 61 g (net). * Solid (A60) 9.2 g (wet) Decanted (A58) at ~20.5 C: * Liquid (A61) 271 g. * Solid (A62) crystal needles 23 g wet. Trying to drain and dry (A62) over napkin and filter paper. Seem to dry well, not deliquescent (but maybe the liquid is). 8.53 g dry! ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-03-01-Wed-s1.txt dimy grass Discarded (A31). Solution (A57) (with water and ethanol) crystallized at ~29 C, white clear needles. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-22-Wed-s4.txt yam anthocyanin Boiling 1 g of (??) dry. Forgot it on stove; may have carbonized. Residue ~3 mm, chalk-like, hard, tan, with a brown thin gooey layer on top. Broke off with some effort. Joined it with (2H) (3H) (4H). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-22-Wed-s4.txt dimy grass Liquid (A13) started to crystallize at 38 C. At 34.5 C, needle-like crystals had formed throughout liquid. Decanted again at ~34 C: * Liquid (A15) * Solid (A16) crystals, 25 g, somewhat thinner and shorter than (A14). Liquid (A15) started to crystallize as it cooled from 34 C to ~30 C. Washed some bits of (A16) with a few mL of (A6). At 41 C (A16) or (A15) was dissolved (but some crystals took a long time to dissolve). Let it cool slowly in a foam jacket (ambient 28.8 C). At 35.5 C, no crystals yet, but seeds did not dissolve. At 34.5 the seeds seemed to grow larger. Lightly swirled at 32 C. Crystals started to form at bottom at 31 C (ambient 27.6 C). After 8 hours (2017-02-25) network of crystal needles similar to ??. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-22-Wed-s4.txt bixin from urucum [Photo: 2017-02-23 03:10] Removed seeds from 32+32+32+34 = 130 g of pods that has been picked about 1 year earlier. Sifted to separate the spines that covered the outside of pods. Result was 73 g of seeds. [Photo: 2017-02-23 04:16] ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-23-Thu-s1.txt dimy grass Decanted (A15): * Liquid (A17) clear light golden yellow. * Solid (A18), 15 g, crystal neeedles 10-30 mm long, thinner than (A16). Total (A14)+(A16)+(A18): 94 g. Should need 116 g of H2O at 60 C. However, dissolved completely at 20 C giving a clear very pale yellow liq. Still unsaturated at 2.4 C. Should have added water more slowly. Either it is a high hydrate, or not NH4H2PO4 at all. Maybe it is DAP not MAP that crystallizes as needles? Cooled (A17) to 19 C, filtered at ~20 C: * Liquid (A21) clear pale yellow. * Solid (A22) mass of small needles. Pressed (A22) between napkins. Heated the moist mass. Melted completely at ~65 C. On cooling at 30 C became a sherbet-like mass of small soft crystals, soaked in light yellow syrupy liquid. Let's see how much water it takes to dissolve at 40 C; then cool to 35 C and decant. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-23-Thu-s3.txt dimy grass Merged (A24) with (A11), the dregs of first dissolution. In (A23), the seeds still did not grow ay 49 C. Seeds started to grow between 47.5 C and 48 C. At 40.5 C, became a mass of crystals immersed in liquid. Decanted between 40.5 C and 40 C: * Liquid (A25) light gold yellowclear, 351 g. * Solid (A26) crystal needles white clear slightly wet, 71 g. Reheated (A25) to 47 C. Left to cool in a foam-jacketed beaker: * At 38.5 C more crystals started to appear. * At 38.0 C a sparse network of crystals formed. * At 37.0 C the network became dense. Decanted at 37.0 C: * Liquid (A27) 312 g, light yellow clear. * Solid (A28) clear white needle crystals, 33 g. Reheated (A27) and put back in a foam-jacketed beaker. * At 36.5 C, seed crystals were just stable. * At 25.5 C started cryst. --- Put 3 g of (A28) in a small beaker covered with majipak and hole. Added 17 g ethanol 99%. Heated in BM to boiling point of ethanol. Needle like crystals were destroyed and bacame crystalline powder (dehydrated?) Decanted hot: * Solid (A31) small crystals, less than 1 g. * Liquid (A32) clear, 17 g. Filtered (A32) through 20 µm paper. Evaporated some on a watch glass; crystals formed. Boiled (A32) in BM. Started at ~78 C, stopped at ~82 C. Still liquid clear. [After cooling tp ?? C], when disturbed congealed instantly into needles. --- Summary of (A23) cooling: * At 47.5 C: 423 g liq. * Between 47.5 C and 40.5 C: 71 g of crystals. * Between 40.5 C and 37.0 C: 33 g of crystals. * Between 37.0 C and 27.0 C: 40 g of crystals. * At 27.0 C: 270 g liq. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-23-Thu-s2.txt Dimy grass Added some H2O o (A22) and heated slightly until nearly complete dissolution. Seems only slightly undersaturated at 38 C. Cooling in jacketed beaker (ambient 31.3 C): Still unsaturated at 34 C. Crystals formed at ~32.5 C. At 32.0 C, mass of very fine needles suspended in clear liq. Dissolving another batch. Plan: use (A6) (now ~350 mL) to dissolve another 250 g of fertilizer at 60 C. The scale reset itself halfway so the total wt is not known. The remainder of the bag is 833 g but certainly more than 168 g were added. Heated (A6) with new load to 60 C. Last grains dissolved at ~58 C. Tan liquid, OD ~5mm with carbon rod. Filtering through snob at 52-55 C into jacketed beaker. Re-boiled the ppt with some filtrate to ~80 C and added back to filter. * Liquid (A23) clear golden yellow, saturated at 51-53 C. * Solid (A24). Re-heated liquid (A23) to 54 C, let cool in jacketed beaker from 53 C. At 50 C put some seed crystals in it. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2017-02-26-Sun-s1.txt dimy grass Decanted (A41) at 26 C: * (A44) a few long needles ~2.60 g * (A45) clear light golden yellow liq; 433 g including E6. Decanted (A22) at 26 C: * (A47) clear very light golden yellow liq; 40 g * (A46) mass of many very small needles, clings to moisture; 21 g moist, 9 g squeezed semi-moist. Merged (A45) into (A47). Merging all crystallized stuff: (A44) 2 g, (A46) 9 g, (A28) 28 g, (A26) 51 g, (A42) 39 g. Result is (A48) 129 g. Trying to redissolve and crystallize all. Must add water slowly since dissolution is very endothermic. To (A48), 129 g, added 3 g H2O = 132 g. At 90 C dissolved almost entirely, with some smell of ammonia. Crystalline film formed on surface. Added 16 g H2O; dissolved entirely at 88 C; 148 g. In a test tube (E5), added some ethanol 92 to sample of (A47). On standing deposited crystals ~2 mm diam, polyhedral rather than needle-like. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-11-Sun-s4.txt cobalt pigment Filtering (ME67s), 20 um paper, washed with ~5 mL (H1) and ~15 mL ethanol 46%: * (ME96) ppt; contains extraneous carbonates. * filtrate merged into (MEF1g) Added 5 mL HAc to (ME1z); still green but cloudy? Heating. Added +2 mL HAc. Formed a fluffy sticky bluish grey ppt that stuck to walls. (Cellulose?) Color became light tan cloudy. Merged (ME95) into (ME93) ("cobalt oxide" neutral). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-12-Mon-s1.txt cobalt pigment Prepared (V1) 10 g HAc + 20 g H2O. Put 2+2+2+3+2+2 = 13 mL of (V1) on the filter paper of (ME96). Eventually started bubbling but then stopped. Some blue liquor was still impregnated in the paper and became black. Final filtrate (ME97) was clear wine-red liq, ppt (ME97) was brown black. The (ME1z) suspension would not settle; still light peack cloudy. Added 1 mL HAc. Tried to boil in large erlen but had to stop because of explosive boiling. The heavier ppt grains became pink. Added 1 mL H2O2 30% to (ME1z). No reaction immediately, but in time the color changed to white cloudy with only a very slight pink tinge, and most of the grainy ppt dissolved. Filtering (MEF1g), the blue liquor extracted from carbonates by (H1): * filtrate (MEF2) two phases: (dark blue clear liq) + (clear white supernat). * ppt (MEF3) brown. The filtrate (MEF2) developed a black ppt in suspension. Washed (MEF3) with 2 mL (V1). Test tube (ME1zp): 1 mL (ME1z), 0.5 mL citric acid sol: no obvious immediate change. Lost the peachy tinge? After ~2 days: (clear white very sly. cloudy liq) + (very small amt of white ppt). Dumped liq in (MF0); discarded the ppt. Added 3 mL ethanol 99 to (ME1xa), and 3 mL ethanol 46 to (ME1xb). All blue color disappeared from both. Formed a black ppt that stuck to glass, and a clear white liq. Finished washing (MEF3) with water into (MEF4); very very light blue clear. Added HAc, Na2CO3 sol, until stopped bubbling; slightly milky. Washed (ME96) with water. Reddish clear wash added to (MF0). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-12-Mon-s2.txt cobalt pigment Refiltering (ME97) (dark purplish red clear liq with some dirt specks) with 14 um paper: * liq (ME98) magenta clear. * ppt (ME99) very small amt; added to (ME96) Refiltering (ME90) (blue liquor with ethanol) with 14 um paper (took forever): * filtrate (ME100) multiphase: (dark blue clear liq) + (white clear liq supernat.) + (bleck ppt in suspension). * ppt on filter (ME101): brownish black, small amt. Scraped off (MEF3) (tiny amt brown-black powder) from filter paper and stored in a 1 mL vial. Put filter paper (MEF3) with 6 mL (V1) in a beaker = (MEF5). After 1 day, (ME1z) was still partly milky but the suspension was turqoise! The coarser ppt was still pink though. Added 1 mL HAc and 2 mL HCit solution. No immediate changes. Acidifying (MD66) (nice medium blue clear liq + very faint white ppt) with HAc. After ~38 mL, blue color of liq disappeared and large cotton-like blue-gray lumps formed. At ~44 mL (pH ~6.5) a dense ppt formed, white with a slight pinkish tint. Added 10 mL NaHCO3 sat sol; no difference. Added 2 mL (H1); brought ph to ~8. Then added 1 mL HAc; brought pH to ~6.5. Suspension had a pinkish tinge. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-15-Qui-s1.txt cobalt pigment Chopped up filter paper with (ME101) (small amt of greenush-brownish black ppt). Put into beaker with H2O to wash off remaining NaHCO3/Na2CO3. Then decanted the liq (clear white) and merged into (MEF5). Pipeted out ethanolic phase of (MEF2) (clear light yellow) as (MEF2p), merged it into (ME1p). Siphoned out the blue liquor phase of (MEF2) (blue sly cloudy) as (MEF2q). Siphoned out supernat of (MD66) (sly peachy, sly cloudy) as (MD66n) (pH ~7). No reaction with K4Fe(CN)6. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-15-Qui-s2.txt cobalt pigment By now (MD72) had dried to a dark rusty-brown solid, 0.35 g. By now (MD66k) had dried to a pinkish tan solid, 0.11 g. By now (ME11) was a tan solid 2.52 g. Merged (MD72)+(MD66k)+(ME11) as (ME11r). Added 4 mL H2O, 2 mL HAc. Some bubbling. Decanted supernat of (ME1z) (sly cloudy); merged into (MD66n). There was some efervescence and the cloudy liq became sly greenish. Heated rest of (MD66) to ~80 C. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-16-Sex-s1.txt dimy grass Descarded (A70) (residue crytallized in bottle from MAP solution). Discarded (H1), (V1). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-18-Dom-s1.txt cobalt pigment In test tube (MH1): a small amount of unprocessed cobalt pigment + 2 mL Na2CO3 sol sat 16C. Heated in BM. No apparent dissolution. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-18-Dom-s1.txt filtering tests Timed filtering of 30 mL water through Kitasato K1 with fresh silicone seals: * gravity alone: 160 sec. * suction with aquarium pump: 5 sec. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-18-Dom-s1.txt cobalt pigment Filtering (ME1z)+(MD66), washed with H2O: * (ME102) liq clear white, very sly pinkish pH 6.5. * (ME103) white sly pink ppt In test tube (ME1zk), the filtrate (ME102) gives white ppt with K4Fe(CN)6. Filtering (ME11r) (cleat dark pink liq + coarse sandy brown ppt) through Whatman 14 um, washed with several mL H2O: * (ME11ra) clear dark pink. * (ME11rb) brown gritty coarse ppt. Pipetted out most ethanolic phases of: * (ME1xa): left ~1.5 mL black suspension. * (ME1xb): left ~0.2 mL black suspension. * (ME1a): left ~0.6 mL blue opaque liq. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-28-Qua-s3.txt cobalt pigment Added 14 mL Na2CO3 (16 C sat sol) to (ME11ra). After bubbling stopped, dirty lilac ppt formed (dirty because of irin content?) Heated to boiling in order to get it to precipitate faster. Decanted supernat of (ME154): light green liquor (ME160). Added again ~50-100 mL of (ME107)+(ME132) to dirty filter papers in (ME154), plus 2 tsp of NaOH. Decanted: blue liquor (ME161)! Added Na2CO3 (solid and sol) to (ME1ps), until stopped bubbling and prescipitated cobalt carbonate as a purplish brown fluffy ppt. Heated to speed up settling. Washed (ME1pt) into filter of filtration ((1)). Added a bit of NaOH to green liquor (ME160). Heated. Remained green but became smokier. Washed (ME131) (very small amt of black ppt) from filter paper with H2O, into filter of filtration ((1)). Chopped the filter paper of (ME131) and added the bits, still partly impregnated with black ppt, to (ME154). Added a bit more NaOH to green liquor (ME160). Still no change in color, but maybe a bit smokier. Both (ME160) and (ME161) have pH ~13.5-14. Filtering the blue liquor (ME161): * (ME162) liq; clear prussian blue. * (ME163) ppt; practically none apart from paper fibers and bits. However the filter paper became impregnated with a greenish-brown liq. Discarded. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-29-Qui-s1.txt cobalt pigment As usual, (ME120) deposited black flakes and crust in the ethanolic phase. The green liquor (ME160) became clear brown, instead of blue. So the blue vs green is not a matter of pH? The blue liquor (ME162) became smoky on standing for a few hours, but was still blue. Washed the black ppt (ME121) with H2O, dumped the wash into alcaline residue flask (MG0). Washed the ppt off the filter into filter of filtration ((1)), that is (ME151). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-28-Qua-s2.txt cobalt pigment Testing dissolution of "oxide" (black ppts) with NaOH solution (H1). Merged black powders (MC20)+(ME9)+(MC18)+(ME108) into a large test tube (ME140). Squeezed liquid off the chopped filter papers (ME1pq) (clear very light pink) into acidic residue flask (MF0). Washed the paper bits with lots of water. Filtering the wash-off as filtration ((1)): * (ME150) liq, clear white, very sly pink. * (ME151) ppt, black. The filter papers (ME1pq) still had some black ppt impregnating them. Put in a beaker (ME154). Squeezed liquid from filter paper bits in (MEF5) and (ME101) (ppt from blue liquor treated with ethanol, filtered out and steeped in HAc). Filtering: * (ME152) liq, clear very sly pink. * (ME153) ppt black. Washed with ~2 mL H2O, with wash merged into (ME152). Squeezed the liquid off the filter paper bits in (ME93) into filtration ((1)), that is, (ME150) and (ME151). Washed the filter paper bits in (MEF5), (ME101) and (ME93) with lots of H2O. Dumper the washout in the filter of filtration ((1)). Added the filter paper bits, still with some black impregnation, to beaker (ME154). Added ~100 mL of (ME107)+(ME132) to the dirty paper bits in (ME154). Heated. Added 1 tsp of NaOH. No obvious blue color. Washed the black ppt (ME153) off the filter paper into filtration ((1)), that is, (ME150) and (ME151). Filtering (ME1pr): * (ME1ps): liq, clear salmon pink. (Contains iron?) * (ME1pt): ppt, brown (Contains iron?) The filter paper bits in (ME1pr) were now almost clean; discarded. Added 8 mL Na2CO3 sol (sat 16 C) to (ME152). After bubbling stopped, lilac ppt formed. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-26-Mon-s2.txt cobalt pigment Residues of (ME1q) (lumped, brow-black), (ME7) (greenish tan), and (ME106) (light pink) treated with 2 mL HAc each. * (ME106) yielded a clear light pink liq + pink ppt. * (ME7) yielded very light tan liq + tan ppt. * (ME1q) yielded very light pink clear liq + gray brown ppt. Added all three (liqs and ppts) to acidic residue flask (MF0). Added 2 mL HCit sol to (ME109). No change. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-27-Tue-s1.txt cobalt pigment Item (ME109) is still (milky light tan liq) + (white fluffy ppt). Probably both are siilica. Fltering (ME100) (blue liquor from fusion, plus ethanol), 14 um paper: * (ME120) liq, 2 phase: (top, clear white ethanolic) + (bot, clear light blue). * (ME121) ppt black. Very slow filtering. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-28-Qua-s1.txt cobalt pigment Filtering (MEF2q) (blue liquor extracted from carbonates with (H1), plus ethanol): * (ME130) liq, 2 phase: (top, clear white ethanolic) + (bot, clear blue). * (ME131) ppt, olive black powder. Filtration was fast. Washed (ME131) with H2O. Wash water (ME132) was clear very light yellow. Added some ethanol 99% to (ME130) and shook. The clear blue phase became smoky. Merged (ME132) and (ME107). Mostly NaOH; pH ~13. Discarded clear white supernat of test tube (MH1), leaving the strong lilac ppt. Added some 2 mL of the supernat of (MF0) and 1 mL of HAc to the ppt of (MH1). Intense bubbling. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-19-Mon-s1.txt cobalt pigment Dumped what remained of (ME1xb) on a paper filter, (ME1xc). Was ~0.5 mL of liquid (2 phases?) with a suspn of black flaky ppt. Washed the test tube with H2O, dumped into (MG0) (basic residues). Tube (ME1xa) stillhad ~1 mL ethanolic liq over ~0.5 mL black sticky ppt. Pipetted out the liq into (ME1p) (ethanolic extracts) and added 4 mL H2O. Result was a suspn of a black ppt. The back crust that was stuck to the tube walls came lose too. Meanwhile (ME1a) and (ME1aa) became (clear liq with very slt yellow fog) + (yellowish gray ppt). The ppt was darker in (ME1a). Decanted (ME1pq) to (ME1pr) rinsing the filter paper bits with some H2O. Added 1 mL of HAc?? to both. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-22-Qui-s1.txt cobalt pigment Merged the white 'silica gel' ppt (white cumbs) of (??) into (MD22). In a tube added a few crumbs of that ppt and 0.5 mL HAc. No bubbling, but the ppt made de a popping sound when it hit the HAc. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-26-Mon-s1.txt cobalt pigment Scraped off (ME108) (brown black powder) from filter paper, saved in small flask. Chopped the paper with some impregnated ppt and added to (ME1pr). Added 5.5 mL HAc to (MD65). Bubbling; dark magenta liq, a bit opaque. Washed out with ~5 mL H2O. Filtering on Whatman 14 um: * (MD100) liq, dark magenta clear. * (MD101) almost no ppt; maybe whitish? Decanted supernat of (ME1q) (clear yellowish brown), (ME7) (clear, sly green), and (ME106) (clear white) as (ME109). Added 35 mL HAc. Lots of bubbling; spilled ~150 mL. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-18-Dom-s2.txt cobalt pigment Prepared (V2) = 10 mL HAc and 10 mL H2O. Washing (ME103) (sly pinkish white ppt, like silica gel) with 9 mL (V2). Washout (ME106) was clear very sly pink. Added 36 mL NaHCO3 sol (sat 30 C): bubbling. Added 8 mL Na2CO3 sol (sat 16 C): bubbling stopped but no ppt. Still clear sly pink (maybe darker?) Discarded (ME102) (clear white). In test tube (ME106k) put 2 mL of (ME106) and 0.2 mL of K4Fe(CN)6. Light tan ppt. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-19-Mon-s2.txt cobalt pigment Stored (ME11rb) (tan grainy ppt) in a vial; 2.38 g. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-20-Tue-s1.txt cobalt pigment Discarded (ME1zk) and (ME106k). Decanted (MD27) (pale pink clear liquor, pH 9.5, lots of NaHCo3/Na2CO3); merged into (ME106) (ditto). Left small amt of pink ppt (MD27p). Heating (ME106). Boiled for ~15 min with silica gel stones to nucleate. On cooling became peachy cloudy with a small amt of pink ppt at bottom. Added 1 mL HAc to ppt; no bubbling, but became stronger pink. Dumped into (MF0). Added 1.0 mL HAc to (MD27p). No immediate reaction. (Must be silica.) Pink tone became more intense after a while. Dumped into (MF0). In (MEF2), the small amt of liquid had no blue left; only a suspn of black flaky ppt in clear white viscous liq. Added ~50 mL H2O. Filtered (MRF2): * (ME107) liq; clear white. * (ME108) black flaky ppt (no silica, hopefully). Decanted the small amount of blue liquor from (ME1a), about 0.2 mL, into (ME1aa). Left behind grayish ppt with some blue liquor. Added 3 mL H2O to both. Became gray syspensions. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2018-03-29-Qui-s2.txt cobalt_pigment Filtering (ME152) Whatman 14 um: * (ME164) liq; very sly pink clear. * (ME165) ppt; lilac. Pipeted out the supernatant liq (clear white) of (ME1xa). Dumped the black ppt (~2mm) into the filtration ((1)), that is, merged with (ME151). Collected (ME165) from filter paper as a gelatinous dark lilac mass. Tried to put into a test tube but stuck to walls. Added 3 mL H2O to wash the walls. Result was a thick suspension that did not settle. Added ~5 mL EtOH 99% in attempt to help settle. Did not work, but suspension became brown-gray. Heated in BM; still did not settle. Filtered (ME11ra) (extract from 'brown' residues with HAc, then precipitated with Na2CO3) through the same paper used for filtering (ME152): * liq merged into (ME164). * ppt (ME166) brownish lilac; washed with lots of H2O. Re-filtering (ME165) (carbonate + H2O + EhOH): * liq (ME167) clear white discarded. * ppt (ME168) dark sly greenish brown. Filtering (ME1ps): * liq (ME169) clear white. * ppt (ME170) orangish light brown. Added 1.5 mL Na2CO3 sol (16 C sat) to (ME164) (clear very light pink). No change. (Maybe the pink hue is a CO2/cobalt complex? Maybe solubte cobalt bicarbonate?) Transferred carbonate ppts to test tubes and added some (H1): * (ME168) (small amt): added 2 mL, turned dark blue. * (ME166) (larger amount): added 4 mL, turned witish med blue, and hot. * (ME170) (a bit larger amount): added 6 mL, turned royal blue, and hot. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-09-22-Dom-sX.txt (T1) 2g EtOH sol CaCl2 (20-25%) + ~10 g H2O (T2) 1.06g Na2SO4 (Da.Neura) + 512g H2O (T1)+(T2) = (NS1) dese white ppt ---------------------------------------------------------------------- Cobalt pigment (MK25) developed a crust of black mold ~2mm thick with white fluff on top. (FCL3) discarded. (FOX3) dry powder white, ~2mm bottom of tube. (FOX1) yellow orange opaque solid in light yellow liquid, (crystals in balls ~2mm diam). (FOX2) Orangish pink clear liq. (FOX9) bright yellow crystals, clear white liquid. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-09-29-Xxx-sX.txt carotenoid pigment from ipê flowers Had collected ~3 L of fresh yellow flowersjust fallen from tree. Left them in fridge for too long (10-20 days) and they turned into a brown wet mass. Put some of it in blender with 150 g EtOH from distillation (ME300h) and 60 g Na2SO4 anhydrous. Strained liquid through double shirtcloth with strong wringing to obtain a brown liquid. Put the liquid back in the blender with more flower mass, blended and strained. Repeated the blending and straining 3 times total. Result: 110 g wet residue (some 50 g lost in cloth etc.) + 216 g dark brown liq qith some white susp solid. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-22-Sat-s1.txt Determining hydration of CaCl2.xH2O Put 20.4 g of CaCl2 hydrated in stainless steel can. Heated on electric stoveuntil stopped fizzling. Turned into 15.2 g of opaque white hard amorphous. So the water content was 5.2 g, consistent with x = 2.1 Added EtOH to make 50.1 g (CA1). Dissolved with difficulty to give sly cloudy white liq. Filtered: * (CA2) clear white liq sly viscous * (CA3) small amt of white ppt. Some dark grains (metallic?) The white ppt (CA3) under microscope is irregular clear white grains; maube silica? The dark grains are spherical opaque. Could be from the cup, which was new with strong manuf scratches on the inside. Solubility of CaCl2 in 100 g EtOH is 25.8 g at 20 C, 35.3 g at 40 C, so interpolating should be ~30.6 g at 30 C. Solubility of FeCl3 in 100 mL EtOH is 83 g (25 C?) ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-24-Mon-s1.txt [CF1] 2 mL CaCl2 in EtOH (CA2) + 0.5g FeCl3 semi-hydrated. Result was orange-brown suspension even near boiling point. Takes a long time to settle; maybe heating makes it more opaque, not less. [CF2] 2 mL CaCl2 in EtOH (CA2) + ??? ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-25-Tue-s1.txt Eventually settled in test tube as black (or dark brown) fine powder ppt, ~2mm; some tiny black crystals on walls; ~40 mm of clear yellow liquid. Decanted most of the liquid from [CF1] to [CF3], leaving ~4 mm with dark ppt in [CF1]. Added 10 mm (in 10 mm diam tube) of EtOH 99% to [CF1] obtaining orangish-brown suspension. Neither [CF1] nor [CF3] changed when hot. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-03-Sat-s3.txt Added 2 mL (OX2) to (MK31a). No immediate reaction. [MK29c] small amt CoC2O4 (pink white susp) + drop of (H5') (NaOH 15%). The ppt turned blue with clear white supernat. With 2 drops, ppt turned pink-gray. Merging [MK29a] into [Mk29b]. Layers of ppt in test tube: from top to bot, clear pink liq, pink ppt, blue ppt, pink ppt, blue ppt. After mixing and heating: pink susp in clear white liq. Merged (MK18e) (clear red) into (MK25). Starting to precipitate all cobalt as hydroxide. (MK31a) (reddish tea clear, maybe lots of iron): added 14 mL (H1) (NaOH 50%). The pH changed from < 5 to > 12 but there was no ppt. The color only became darker tea. (MK25) (cobaltred clear): added 4 mL (H1). Blue ppt formed immediately, pH 4.5. Merged [MK29c] into [MK29b]. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-04-Sun-s1.txt Added 14 mL (H1) to (MK25). Turned dark blue susp in clear pink liq. Then turned greenish dark blue. Added 12 mL (H1) to (MK25). Pipeted out some supernat (clear white) of [MK29b]. Added 0.5 mL NaOH 15% (H5''). Still pink suspension (darker than CoC2O4). ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-05X-Mon-s1.txt [MK29b] Three layers in test tube. From top: clear liq, dark brown (CoOOH?), pink (Co(OH)2?) (MK25) Three layers in big erlen: very light pink clear liq, ~2mm green ppt, ~50mm greenish blue ppt. (FOX9) Developed light yellow crystals at bottom. Supernat is very light yellow clear. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-01-26-Sat-s1.txt (After long gap previous 2018-10-22.) cobalt pigment (MK2) was supernatant (light blue) of fusion and dissolution (MK1) of cobalt pigment + NaOH, done on 2018-09-14. Currently it became a clear supernatant + dark olive ppt. Filtering by gravity: * (MK2p) olive-black ppt * (Mk2q) clear white liq (may contain xNa2O.ySiO2) slightly olive smoky. (MK3) was supernat (clear white) of (MK1). Now clear liq with long crystals (Na2CO3?) +some black powder ppt. Decanted the liq from (MK3) -- clear, sly olive smoky, viscous -- to(MK3q) Crystals (MK3p) washed with a bit of EtOH 46%. With acid, (MK3p) everfesced, but left a white ppt (SiO2?) (MK13) and (MK13a): mass of wet crystals, white, semi-opaque. With HCl, it bubbles but leaves behind a small amt of crystalline opaque solid. Merged (MK13a) (MK3p) into (MK13). Dried on petri over warm heat; left mass of white crystals. Added ~70 mL EtOH 96%. ---------------------------------------------------------------------- Discarded (MK2a) (MK3a) from watchglass. Old (MK1b): clear, with a bitof ocher ppt. New (MK15): clear liq with brown-ocher ppt. Merged (MK1b) and (MK15); filtered: * (MK20) clear liq. * (MK21) brown ocher ppt; probably Fe more than Co. (MK1d) (was (MK1) + H2O + Na2S2O5 + HCl): pink-tangerine liq + white ppt. Pipeted out supernat (~5 mL?) to (MK17). Resuspended the ppt with some H2O. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-01-26-Sat-s2.txt [MK18a] (was (MK18) + HCl): clear light pink liq. [MK18b] (was (MK18) + HCl + Na2S2O5): clear pink liq. [MK18c] (was (MK18) + Na2S2O5): clear pink liq + white ppt (CaSO4?). Merged supernats of [MK18a] [MK18b] [MK18c] into (MK17). ---------------------------------------------------------------------- (MK18) (was cobalt hydroxide ppt filtered from MK14): greenish dark gray powder (with fibers?). Resuspended in H2O. Merged with (MK2p) (dark olive brown ppt). Added 10 mL HCl 20%. Result was black suspension. After 10 hours, separated into dark red liq, pH 4, and black ppt. ---------------------------------------------------------------------- Collected alldirty filter papers in erlen (MK23). Covered with H2O + 10 mL HCl 20%. Some bubbling. After 10 h, light clear pink liq, pH 1.0-1.5. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-01-27-Sun-s1.txt Added 2 mL Na2S2O5 sol 25% + 8 mL HCl 20% to (MK18). No immediate change. Added 2mL Na2S2O5 sol 25% to (MK23) too. No immediate change. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-01-Thu-s1.txt Merged (MK16) (dark red-pink clear), (MK17) (pink clear) and some supernat of (MK18) (dark pink) to (MK23). Filtered (MK23) to remove paper bits, added filtrate to (MK25). Put paper filter with traces of (MK18) plus the filter paper with (MK21) (small amtblack ppt) into clean erlen (MK26),with H2O and ~8 mL HCl 20%. Prepared another batch of (H1), NaOH 50%. Namely, 95.6 g NaOH + 96.6 g H2O. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-02-Fri-s1.txt [MK7a]: gray wet ppt. Was some supernat treated with HCl. Merged (MK10) into (MK9). Both are very light blue powders (SiO2?). Discarded the white ppt of [MK18c]. Merged (MK1ab) (blue silica?) + (MK9) + (MK10) + (MK7a) in erlen (MK27). ---------------------------------------------------------------------- Dumped [Mk7b] (black ppt + light blue supernat) + H2O to erlen (MK28) (olive brown susp). Added 8 mL HCit 58% sol. Result: brown susp. Filtering (MK18): * (MK18l)dark pink liq. * (MK18p) ppt brownish translucent fibrous; may be paper fibers. ---------------------------------------------------------------------- Prepared another batch of HCl 20% from HCl 37%. To each gram of HCl 37%, one must add 0.85 g H2O. Cooled HCl 37% and empty bottle in ice bath. Added 101 g HCl 37%, 85 g H2O ---------------------------------------------------------------------- Added 2 mL HCl 20% to [MK14a]. Originally gray blue ppt, treated with glucose, now brown ppt. Turned into pink sol, with ppt of mold. Added 2 mL HCl 20% to [MK14b]. Same origin, but with NaAsc instead of glucose. Darker orange solution. Filtered (MK1d): * supernat very sly pink, added to (MK25) * white sandy ppt, added to (MK27) Discarded [FR2] [FR3] [FR1] (had dried up). [FS4] (iron acetate) had dried to dark orangish black solid. Added H2O. Redissolved almost completely to clear dark orange liq. [FS5] (iron lactate) still dark yellow solution. In [FOX1] put 1 g FeSO4.xH2O dissolved in H2O. Milky light yellow solution. Added ~4 mL H2O2 dropwise; lots of bubbling, turned into orange-ocher suspension. ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-02-Fri-s2.txt Trying to use oxalate complexation to separate Fe from Co. Theory: Fe(III) oxalate is sluble, Fe(II) is insoluble (yellow) and Co(II) oxalate is insoluble (light yellowish pink). Added to [FOX1] 1.5 g NaHSO4. Turned pale yellow almost clear, pH 1.5. Prepared [FOX2]: 1.00 g CoSO4.yH2O + 30 mm H2O. Orangish pink clear sol. Prep [FOX3]: 1.00 g Na2C2O4.zH2O + 40 mm H2O. Clear, but left undissolved ppt at bottom. Prep [FOX13]: 1 mL [FOX1] + 2 mL [FOX3]. Changed from very light clear yellow to clear yellow. Prep [FOX23]: 1 mL [FOX2] + 2 mL [FOX3]. Changed from clear pink to clear white + pinkish white ppt. Added 1 g NaHSO4 to [FOX2] to incease acidity. pH 1.5. Still clear pink. Prep [FOX23']: 1 mL [FOX2] (with the extra NaHSO4) + 2 mL [FOX3]. Same as [FOX23]: clear white liq, pinkish white ppt. Prep [FOX123]: 1 mL [FOX1] + 1 mL [FOX2]. Result clear tangerine liq. Added 6 mL [FOX3]. Right away, just clear golden yellow liq, no ppt! 8-( However, ppt started to form after a couple of minutes. After an hour, clear yellow liq + pink white ppt! 8-) ---------------------------------------------------------------------- ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ #FILE 01-Notebook-Split/2019-02-03-Sat-s1.txt Filtering [FOX23] + [FOX23'] + [FOX123]: * (MK29) ppt pinkish white (CoC2O4) * (FOX9) clear pale yellow liq (Fe2(C2O4)3) ---------------------------------------------------------------------- Evaporating supernat of (ME461) on petri dish (MK30) (was CoCl2 in EtOH; clear purplish blue). Added 1 mL HCl 20% and some H2O to remove the pinkish white crust at bot of flask. Discarded? Left in (ME461)? ----------------------------------------------------------------------