#FILE .discard # Last edited on 2019-11-20 12:51:46 by jstolfi GALLEY TRANSCRIPT OF LAB NOTEBOOKS This text should be moved to the notebooks of individual experiments. ---------------------------------------------------------------------- 2019-02-03 Sat [2] Noted (ME53b) was a tea-colored liq with a hard crust of clear largish white crystals at bottom of the erlen. The crust was ~2mm thick and bulged up in the middle, separating from the erlen bot. It was very hard to remove but broke down immediately once the outer rim (that pressed against the erlen wall was breached. Decanting/filtering (ME53b): * (MK31) liq tea-colored * (MK32) crystals Merged [FOX13] into [FOX9] (clear light yellow). Filtering (MK28) * (MK33) liq tangerine clear * (MK34) small amt of black flakes; dumped into (MK26) Added (MK461) (susp of white ppt in pink clear liq) to filter of (MK18). Put rest of crystals from (ME453b) on a petri dish to dry (ME501). Added 6 mL Na2C2O4 sol conc to (MK33) (tangerine clear liq). No immediate change, not even on heating. After EtOH of (MK30) -- old (ME451) -- evaporated, merged into (MK25). Noted (MK33) slowly becoming cloudy and pink rather than tangerine. Refiltering (MK31) * (MK31a) liq clear dark tea * (MK31b) ppt Added some EtOH from distillation (ME300h) to (ME501). Preparing (OX2) concentrated solution of H2C2O4 (HOxa) in H2O that is saturated at 35 C. Prep [MK29a]: small amt CoC2O4 (pinkish white susp) + 1.5 mL HCl 20%. Result: pink clearliq. Prep [MK29b]: small amt CoC2O4 (pinkish white susp) + 2.0 mL NaOH 50% (H1). Result: blue clear liq + ppt. ---------------------------------------------------------------------- 2019-02-25 Tue [2] Test tube [CF2] dropped and broken. Lost contents. ---------------------------------------------------------------------- 2019-03-03 Sun [1] Trying to get an approximate value for solubility of FeCl3 (anhydrous) in EtOH (anhydrous). ---------------------------------------------------------------------- 2019-02-15 Tue [2] Test tube [CF2] dropped and broken. Lost contents. ---------------------------------------------------------------------- 2019-03-03 Sun [1] Trying to get an approximate value for solubility of FeCl3 (anhydrous) in EtOH (anhydrous). (FCL0): Heated 30g EtOH 99.3% (Quimisul) at ~60 C. Dumped in ~10g FeCl3 partially hydrated (Implastec) Bubbling (HCl?) Brown-orange suspension. Washed beakers with EtOH 99% but had absorbed some water. Orange-brown fine powder suspended in yellow (?) clear liquid. --> (FCL1) Filtering (FCL0) with whatman at 25 C: * liq (FCL2) clear dark orange, sly smoky (brown s??) * ppt (FCL3) orangish-brown, small amt. Ocher when dry. < 0.05 g Washing ppt with EtOH 99%. Wash (FCL4) is clear orange. Heating (FCL2) in BM from 25 C to ~50C. At ~45 C some droplets formed on the wall of the erlen above the liq. Seemed oily rather than EtOH. At 50 C the(FCL2) did not become clear. May have become more opaque. Maybe continued hydrolysis/ethanolysis. Cooled (FCL2) to 25 C. Totally clear liq with orange-brown ppt at bottom. ---------------------------------------------------------------------- 2019-03-04 Mon [1] Refiltered (FCL2): * ppt (FCL5) ocher; almost nothing. * liq (FCL6) dark orange clear ---------------------------------------------------------------------- 2019-10-14 Mon [1] [AT13a] bit of (AT13) (dark red) + ~1 mL ethyle acetate: insoluble. [At13b] bit of (AT13) (dark red) + ~1 mL EtOH 99%: insoluble too. [At13c] bit of (AT13) (dark red) + ~1 mL acetone: sly sol. Thus the red ppt from fermented purple yeam juice treated with acid is only very sly sol in acetone. How can we improve the solubility? Filtering (AT1f) (much slower): * liq added to (AT12) * ppt (AT13') Transposed acetone Nox '500 mL' (Acetona PA ACS, Lote 7096, Fab 07/2016) from plastic bottle (PE with bung; leaky,could smell it) to amber glass. Weight of acetone in old bottle = 367 g (tare 44 g wo bung and stopper). Weight of acetone in new bottle = 368 g (tare 164 g wo bung and stopper). Density [Wikipedia] 0.7845 g/mL at 25 C). Expected weight of 500 mL = 392 g. So ~25 mL were lost since bottling. ---------------------------------------------------------------------- 2019-10-21 Sat [1] Discarded [AT13a] [AT13b] [AT13c] [AB201] [GL1] Prepared sol HOxa (OX5): 0.66g H2C2O4 + 4.11 g H2O. Discarded all but 2 mL used below. More tests with (AT1) fermented purple yam juice and acids: [AT1h] 2 mL (AT1) + 2mL NaHSO4 sol 33% (NAH1): milky dark red. [AT1i] 2 mL (AT1) + 2mL HAc 100%: almost clear dark red bubbling. [AT1j] 2 mL (AT1) + 2mL HcL 20%: clear red milky. [AT1k] 2 mL (AT1) + 2mL HLac 85%: almost clear dark red. [AT1l] 2 mL (AT1) + 2mL Hoxa (OX5): milky clear read. Heating those test tubes in BM to boiling for many minutes. [AT1h] red ppt + dark pink liq [AT1i] homog dark wine sly cloudy [AT1j] red ppt + clear pink liq [AT1k] homog dark wine sly cloudy [AT1l] red ppt + clear dark pink liq So it seems that HAc 100% and HLac 85% cannot precipitate the red stuff. In fact they seem to dissolve it. Not low enough pH? Another test: [AT13q] = some (AT13') (red ppt from NaHSO4) + ~1.5 mL H2O ---------------------------------------------------------------------- 2019-10-13 Dom [1] Preparing (NAH1) = 1:3 sol of NaHSO4 = 50 g NaHSO4 as received (hydrated?) + 100 g H2O. Sol is sly milky. (Calcium in water?) Had to filter it. Small amt of white ppt discarded. Anthocyanin from purple yam After 24 h, [AT1a] was about 15 mm of carmine red powdery lumpy ppt + 30 mm supernat clearlight pink sly cloudy. Moe tests of (AT1), fermented purple yam juice, with varying amounts of NaHSO4: [AT1b] 4 mL (AT1) + 0.5 mL (NAH1). [AT1c] 2 mL (AT1) + 0.5 mL (NAH1). [AT1d] 2 mL (AT1) + 2.0 mL (NAH1). [AT1e] 2 mL (AT1) + 1.5 mL (NAH1). In all four, color turned from wine to red with sly bubbling. Upon heating with blowdryer, the red matter precipitated powdery ppt. The gas volume for [AT1b] was ~1mL. After ~1 h, the four look similar except that the liq in [AT1b] had a stronger pinkish color and was sly cloudy. Since (GL1) did not show any signs of enzymatic activity (bubbling), discarded the yeast culture filtrate (AT9). Heeating [At1a], [At1b], [At1c], [At1d], [At1e] (test tubes), also (AT1b) (erlen), in BM. Heatng makes the red ppt coagulate into a lumpy spongy ppt and release gas. This goes also for [AT1a], 24 h after preparation. Merged [At1a], [At1b], [At1c], [At1d], [At1e] (test tubes), also (AT1b) (erlen) and filtered, washing with ~20 mL H2O: * liq (AT12) pink alm clear. * ppt (AT13) bright red lumpy. Noticed that the self-fermentation of (AT1) caused it to separate into ~60% dark wine-purple gelatinous mass at the top, flowing like egg white; and ~40% pink sly cloudy liq below. Put ~400 mL of the gelatinous mass of (AT1) into (AT1f). Added 10 mL (NAH1); gelatinous mass broke up and became bright red. Heating in BM. Meanwhile the dry solid residue of hand-squeezing the ground purple yam, left over from perparation of {AT1), was light bege dry coarse flour. Discarded. Coloring from ype flowers After 2 days, (YP4) is yellower than (YP3); both clear. ---------------------------------------------------------------------- 2019-10-07 Mon [1] Anthocyanin from purple yam Preparing a yeast culture (AT8) to try to use to remove the sugar groups from the pigment. In a large white plastic jar, added: * 1000 g H2O. * 0.60 g of NH4H2PO4 (A200) as N+P nutrient(?) * 5.0 g of sacarose. * 10 g of Fleischmann's dry yeast. Ambient temp 26 C. ---------------------------------------------------------------------- 2019-10-11 Fri [1] The culture (AT8) has been left for 6 days. Not a good idea. It got rotten, with a disgusting smell. Making another batch (AT10). In another large plastic jar, added: * 1000 g H2O. * 0.30 g of NH4H2PO4 (A200) as N+P nutrient(?) * 5.0 g of sacarose. * 10 g of Fleischmann's dry yeast. Tartar from grape juice Got a cluster of large crystals (wine-colored thin plates, ~10 mm diam) from a bottle of 750 mL of grape juice (Casa Bento) kept in fridge. Weight 5.25 g dry. Added to previous collection (TT1). Pigment from ype flowers Testing the EtOH extract of half-rotten flowers (YP2) with acid and base: [YP3] 1 mL of (YP2) + 1 drop of HCl 20%: clear orange brown. [YP4] 1 mL of (YP2) + 1 drop of NaOH 1:1 (H1): brown milky. After 24 h, [YP4] became clear orange brown,like [YP3] ---------------------------------------------------------------------- 2019-10-12 Sat [1] Anthocyanin from purple yam Testing the effectiveness of (rotten) yeast culture filtrate (AT9): In test tube [GL1], put 1 mL H2O + a bit of glucose + 1 mL (AT9). Clear white sly cloudy; no immediate reaction. Prepared solution (NH1) = 2.5 g NaHSO4 + 5.0 g H2O (total ~5.5 mL). Testing fermented purple yam juice (AT1), wine-purple gelatinous liq, with sodium bissulfate: Test tube [AT1a] = 2 mL (AT1) + 1 mL (NH1). Heated with blowdryer. Separated red clumpy ppt + clear liq. ---------------------------------------------------------------------- 2019-09-29 Sun [2] Added EtOH 26 g from (ME300h) to wash beaker etc. Total 242 g of brown liq (YP1) Anthocyanin from purple yams New batch Bought 5 purple yams at Dalben. Weight after peeling: 225 + 184 + 168 + 147 + 125 = 849 g. Cut into half- and quarter-cylinder slices , 10-11 mm thick. Split into 4 batches of ~214 g each. Blended them slow and fast for several minutes. Strained the puree through two layers of T-shirt cloth, wringing manually, to produce dark wine-purple liquid and a fibrous residue (AT8a). Some white starch quickly settled out of the liquid. Batch (1) ~214 g yam + 150 g H2O. Blended ~2+0 min. Strained, liq to (AT1a). Batch (2) ~214 g yam + 150 g H2O. Blended ~2+2 min. Strained, liq to (AT1a). Batch (3) ~214 g yam + 150 g supernat of (AT1a). Blended ~2+2 min. Strained, liq to (AT1b). Batch (4) ~214 g yam + 150 g supernat of (AT1a). Belnded ~2+2 min. Strained, liq to (AT1b). Residue (AT8a) is light brownish-pink-lilac fibrous mass. Sly moist wt 255 g. Joined (AT1b) and rest of (AT1a) into (AT1c). Re-strained (AT1c): * liq (AT1), wine-purple * ppt small amt, like (AT8a), discarded. Blended again (AT8a) + 600 g H2O for ~2+2 min, pink-lilac paste. Strained: * liq (At2a) wine-purple, lighter than (AT1). * ppt (AT8b) pink-lilac residue; total 236 g moist. Re-strained (AT2a): * liq (AT2) wine-purple, lighter than (AT1). * ppt small amt, like (AT8a), discarded. Blended again (AT8b) + 600 g H2O for ~2+2 min, light pink-lilac paste. Strained: * liq (At3) brownish-pink. * ppt (AT8) light pink-lilac residue. Let (AT1), (AT2), (AT3) decant. ---------------------------------------------------------------------- 2019-09-30 Mon [1] Anthocyanin from purple yam Juices (AT1), (AT2), amd (AT3) developed statch deposits. Decanted supernats of (AT1) and (AT2) into two green glass bottles, put in fridge. Discarded supernat of (AT3). Resuspended starch from (AT1), (AT2), and (AT3) in ~100 g H2O each, as (AT4), (AT5), and (AT6). Left to sediment again. ---------------------------------------------------------------------- 2019-10-01 Tue [1] Starch sediments (AT4), (AT5), and (AT6) were discarded by Patti. ---------------------------------------------------------------------- 2019-10-06 Sun [1] Discarded the rinds of purple yams. Pigment from ype flowers The residue (YP0) from straining the EtOH blended flowers was grayish brown friable; dry wt 61g. Paper "chromatography" of strained EtOH liq (YP1) on filter paper showed a single broenish-yellow component in liq with tan ppt. Stain was not affected by HOxa sol but maybe sly changed by NaOH sol (although it did affect the filter paper more). Filtering (YP1): * liq (YP2) clear dark brown, almost black * ppt (YP3) brown-black paste Discarded (AB200) Sample (FOX1) liquified at 30 C into canary yellow susp. Cobalt pigment Removed layer of mold(?) (MX1) that was growing on top of the supernat of (MK25). ---------------------------------------------------------------------- 2019-11-02 Sat [1] Discarded (AT10); nauseating smell. Black mold colony was floating on top. Checking test tubes with samples of (AT1) with acid: * [AT1h] no change: clear light pink liq, red spongy ppt. * [AT1i] evaporated ~2 mL; still wine-red clear liq, very small amt ppt. * [AT1j] liq clear light brownish pink, red spongy ppt. * [AT1m] clear pink liq; powdery red ppt. * [AT1k] clear red liq, no ppt. * [AT1l] clear pink liq + spongy ppt. Also checked test of (AT13) dry solid resuspended in HAc 100%: * [AT13q] about 0.5 ml supernat clear red + ~3.5 mL susp wine-black ppt Erlen (AT1y) clear sly pink supernat + dark red powdery ppt. In [FOX1]: clear pale yellow liq + ~1 mm yellowish-white ppt In [MK14a]: ~1 mL clear green-yellow liq + small amt gray(?) ppt. Filtering (AT13): * liq (At14) clear pink. * ppt (AT15) red lumpy paste. Discarded (AT1x'). Checking status of (MK25), cobalt "hydroxide" preparation,left standing for months in big erlen with a non-hermetic cover: * Supernat liq, 50-70 mm, very very light pink clear. * Layer ~1 mm of greenish tan on top of ppt. * Bulk of ppt, 50-10 mm, is still bluish-grayish green. No signs that it will setlle more. Pipeted out clear light pink supernat of (MK29) and [MK29b], ~2.5 mL, into (MK26) (acidic cobalt residues): * (MK29): ~1 mL liq, 2mm white ppt. * [MK29b]: ~2.5 mL liq, ~15 mm fluffy powdery light pink ppt. ---------------------------------------------------------------------- 2019-10-19 Sat [2] Discarded [FOX3] (Na2C2O4; now dry powder). Merged [FOX2] (CoSO4 sol) into (MK26) (cobalt residues acidic). Checking [MK29b]: dry residue in test tube, ~10 mm pinkish gray at bottom, 5 mm black at top. Added 3 mL (NAH1) (sodium bisulfate sol 33%). Vigorous bubbling. Result: brown black fine susp. Checking [MK14b]: dry residue, very dark brown film on wall, ~25 mm. Added 3 mL (NAH1). No bubbling. Result: brown black fine susp. Checking [MK14a]: clear yellowish-green liq + grey(?) flaky ppt. Discarded (BT2), [FCL1] (FeCl3 + EtOH), [CF1], [CF3], (YP3), (MK18p) (filter paper). Merged (MK27), (MD22), (MK33b) in bottle: silica(?) from cobalt pigment. Redissolved (MK33) (clear pink gelatinous crust) in H2O. Added 10 mL (H1) (NaOH). Clear blue liq, no ppt! The next goal is to see whether the red ppt from purple yam juice, fermented and treated with NaHSO4, will redissolve in HLac, which does not precipitate it out. So, pipeted out most of light pink supernat (~4 mL) of [AT13q], leaving ~1 mL red ppt. Added 2 mL HLac 85%. Got darker and released many small bubbles. result was a dark wine suspension that did not easily settle. Tried to filter some (AT1) in a coffee filter with a paper towel: * liq (AT1x) pink clear, discarded. * ppt (AT1y) dark wine-colored gelatinous mass. Added 4 mL of (NAH1) (sodium bisulfate) to filter. Color changed to red. Discarded (AT2) since it had developed mold. Filtering [MK33]: * ppt (MK33y) discarded. * liq (MK33z) clear lt blue liq. ---------------------------------------------------------------------- 2019-10-26 Sat [1] Anthocyanin from yam Added rest of filtered fermented yam juice in coffee filter * liq (AT1x') discarded * ppt (AT1y') dard red; infested by small fly maggots. Added to (AT1y). Added 10 mL more of (NAH1), NaHSO4 sol, to (AT1y). ---- Yelloy pigment from small coconuts On 2019-10-16, I collected ~500 mL of small yolk-yellow coconut fruits from a palm tree near IME-USP. The fruits are fig-shaped, 20-25 mm long. Their pulp is ~3mm thick,yolk-yellow, fibrous, with a sticky juice and s strong nauseating sweet smell. Inside there is a small teardrop-shaped coconut, with a thick brown very hard shell. I couldnot remove the pulp easily, not even from the over-ripe fruits. So I tried to boil them for a while. ---- Checking [AT13q]: about ~5 mm clear dark red liq on top, ~30 mm red-black opaque suspension. Rest of (AT13) -- dry whitish red ppt -- put in bottle. Transferred 2 mL of [AT1i] = (AT1) + HAc to test tube [AT1m]. Added 2 mL HCl 20%. Became light bright red cloudy. ---- Checking [MK29b]: pink clear liq on top, pinkish white ppt. ---- Added 2 mL (NAH1) (NaHSO4 sol) to [MK29] (~2 mm pinkish white dry ppt), mixed. Result is pink suspension. Discarded (NS1) (calcium sulfate test). ---------------------------------------------------------------------- 2019-11-02 Sat [3] Combined ppts of (MK29), [MK29b] into (MK29). Washed with ~3 mL H2O; wash into (MK26). Adding (H1) (NaOH 50%) to (AT12) (clear strong pink, ~200 mL). Added2 mL: no change. Added 2 mL more: turned dark black-green opaque (pH 12). After 12 h turned clear orange-brown. ---------------------------------------------------------------------- 2019-11-03 Sun [1] In [AT12u], put 2 mL (AT12) (clear orangish-yellow brown) and 2 mL HCl 20%. Returned to very light clear pink. Checking [YP3]: had evaporated to ~0.5 mL. Clear brown liq, ~1 mm white(?) ppt. Checking [YP4]: had evaporated to ~0.3 mL. clear orange yellow liq, no ppt. Added 4 mL HCl 20% to (YP2). No immediate change. ---------------------------------------------------------------------- 2019-11-10 Dom [1] Pipeted out the supernat of (MK25) to (MK25a), ~370 mL, very pale pink clear. In (MK25), there is a layer of greenish gray mold over the blue-green ppt. Scooped off some of it as (MK25b). Seems filamentous, livid yellowish green. Filtered (MK25a) to remove some bits of mold. Added several tens of grams of NaHSO4 solid to (MK25) until color changed from blue-green ppt to brown-gray then to red opaque. In this last phase, there was substantial small bubbles. Added some Na2CO3 sol to (MK25a). Became cloudy with a pink-lilac ppt. Started filtering (MK25): * liq (MK226) clear dark wine-red * ppt (MK227) ?? ---------------------------------------------------------------------- 2018-10-22 Mon [1] Resuspended some (MK18) (dark greenish olive ppt) on H2O. Created [Mk18a] ?? mL (MK18) + 1 mL H2O (olive-gray susp.) + 1.5 mL HCl 20%. Suspension turned pinkish, less opaque. Created [MK18b] ?? mL (MK18) + 1 mL H2O + 1.5 mL HCl 20% + 1.0 mL sol Na2S2O5. Result was clear pink liquid. Created [MK18c] ?? mL (MK18) + 1.5 mL sol Na2S2O5. Brown susp. in pink-orange liq. Created [MK18d] ?? mL (MK18) + 1.5 mL H2O. Result is just dark olive-gray susp. LONG PAUSE UNTIL 2019-01-26 ---------------------------------------------------------------------- 2019-11-10 Sun [1] Filtering (MK25a): * (MK228) liq clear white discarded * (MK229) ppt lilac turned lilac-grey Checking (MZ1) in amber bottle with stopper: now clear liq + dark ppt + clear white fine needles, easily suspended in liquid. Washed (MK229) wih ~1.5 mL (NAH1). Fizzled and dissolved completely into clear pink liq. Merged into (MK26). Poured (MZ1) into erlesn; suspension opaque greenish-brown. Added tens of grams of solid NaHSO4. A bit of bubbling. Color changed slightly to opaque reddish brown-gray. Added a couple of grams of Na2S2O3 (sodium hyposulfite or sodium thiosulfate) to (MZ1). (Bad idea? should have used metabisulfite Na2S2O5?) Color changed slowly to brown-gray, then yellowish-green gray, then pastel green, always opaque. On standing (MZ1) became a peach milky suspension and a pastel turquoise-green ppt. Pipeted out the tan suspension to (MZ2). Smell of SO2. Washed the pastel-green ppt of (MZ1) with H2O; Saved wash as (MZ3). Transferred ppt (MZ1) to a centrifuge tube. Added 2.5 mL H2O2 30% to pastel-green ppt of (MZ1). Color turned immediately purplish brown with slow bubbling. ---------------------------------------------------------------------- 2019-11-11 Mon [1] Checking (MZ1): still bubbling. Checking (MZ2): almost clear light tangerine with small amt of pastel yellow-green ppt. ---------------------------------------------------------------------- 2019-11-13 Qua [1] Checking (MZ1): bubbling stopped. About 6.5 ml total. Grayish chocolate ppt at bottom; darker chocolate ppt over it; ~4 mL clear white liq; very thin layer of hydrophobic pinkish-white powder on surface and tube walls. Checking (MZ2') clear light tangerine liq +small amt of greenish-white ppt. Checking (MZ3): clear white liq + small amt of pastel green ppt. Washed (MZ227) with H2O a couple of times; wash into (MK226). Result is a ocher-tan paste. Checking (MK226): clear dark red liq, ~700 mL. Filtering (MZ2'): * liq (MZ4) clear light tangerine pH ~1. * ppt (MZ5)small amt pastel yellow-green. Heated a small amt of (MZ5) to red heat with a small blowtorch. Briefly turned into ember, released acrid smoke. Left a light gray powder residue. No reaction with HCl 20%; silica? Discarded. Filtering (MZ3): * liq (MZ7) clear white; discarded. * ppt (MZ8) pastel turquoise-green. Added 3 mL H2O2 30%to filtrate (MZ4). No bubbling. Still clear;maybe slight hue change to light orange instead of light tangerine. Smell of H2S2? Added 6 mL of (H1) (NaOH 50%) to {MZ4). Intense bubbling and formation of an olive-black ppt with slightly olive clear supernat. pH ~13-14. Added 1.5 mL (H1) to (MK226). Formed a royal blue ppt that did not redissolve; pH ~4.5. Added ~10 mL (NAH1); still not completely redissolved. ---------------------------------------------------------------------- 2019-11-13 Qua [2] In test tube [MK226a]: 6 mL (MK226) supernat (clear dark pink) In test tube [H3]: 1 mL (H1) + 9 mL H2O. Added 2 mL of [H3] to [MK226a]. Immediately formed a royal blue ppt that after less than 1 min turned bluish green throughout. A small amt of the ppt that stuck to the wall of the tube turned olive-brown. In test tube [MK226b]: 6 mL supernat of (MK226) + 3 mL of (CO2) (Na2CO3 sol sat 16 C). Dense pink-lilac ppt formed immediately. ---------------------------------------------------------------------- 2019-11-14 Qui [1] Added 4 mL (NAH1) to (MZ4); brought pH down to ~6. Result is very light olive-green liq + olive-black ppt. Checking [MK226b]: separated into three layers of equal height: top and bottom lilac-purple ppt, middle layers dark purple much darker than (MK226); probably opaque. Remixed all. Checking [MK226a]: very light pink clear liq at top, most still bluish-green ppt. Filtering (MZ1): * liq (MZ9) clear white discarded. * ppt (MZ10) chocolate brown. Added 5 mL of (NAH1) to (MK226). Had to squish the lumps of blue ppt to get them to dissolve. pH ~3.5. Checking [MK226b]: clear white liq + grayish purple ppt. Returned [MK226a] and [MK226b] to (MK226). Dissoved completely; pH ~4. Added 2 mL (CO2) (Na2CO3 sol sat 16 C) to (MK226), dropwise. A lilac ppt forms but eventually redissolves; pH ~4.5. Stored the bismuth chloride solution (BI1) in a brown bottle. Prepared more (H1) with 120 g H2O + 120 g NaOH (Asher). After bubbles cleared, result was clear sol, quite hot. Stored without filtering in PE bottle with rest of previous batch (~30 mL). ---------------------------------------------------------------------- 2018-10-12 Fri [1] Heating (MK14) (greenish blue gray susp) in BM. Filtering (MK13) + (MK15): * liq (MK13a) clear white. * ppt (MK13b) brown from (MK13), olive gray from (Mk15). Pipeted out supernat of [MK7a] (~1.5 mL clear light pink) and added some drops of (H5). Added the suspension to the filtration above. Trying to evaporate (MK13') and (MK13a) in a tray under the sun. Added 0.5 mL HCl 20% and 0.5 mL H2O to what was left of [MK7a]. Result was pinkish liq with white(?) gritty ppt. ---------------------------------------------------------------------- 2018-10-13 Sat [1] Added (MK13b) to (MK14). Washed and pipeted out supernat from (MK14) (greenish-gray susp) as (MK15). Trying to redissolve (MK14) again with HCl 37% (cooled to ~0 C to reduce evaporation). Added 10 g of glucose and 1.0 g of HAsc to counteract formation of cobalt(III). After adding ~10 mL of HCl 37% got a black ppt susp. in pink clear liq; pH 5.5. ---------------------------------------------------------------------- 2018-10-14 Sun [1] Pipeted out supernat of (MK14) to (MK16); clear dark red. ---------------------------------------------------------------------- 2018-10-15 Mon [1] Filtering rest of (MK14): * liq (MK17) clear dark red. * ppt (MK18) dark gray green ppt. Dismantled a Panasonic alkaline AA battery: * (PA1) dark rusty brown powder. * (PA2) white paste. Saved ~28 mm of steel casing as handy tube. ---------------------------------------------------------------------- 2019-11-14 Qui [2] Prepared another batch of (NAH1) with 80 g NaHSO4 (Auros) + 160 g H2O. (Barely dissolved in 120 g H2O, so increased to avoid cryst in winter). Had to filter to remove fine white dust (CaSO4?) and some black specks. ---------------------------------------------------------------------- 2019-11-16 Sab [1] Evaporating (MK20) + (MK11) (clear white, pH 9.5) on warm petri. Filtering (MZ4): * liq (MZ11) clear light greenish yellow * ppt (MZ12) olive-black. Decanted (MK26) (wash of colbalt filter paper strips) clear pink, some paper bits. Checking (OX2) (oxalic acid sol): had dried out as crystals clear. Dissolved in H2O to ~80 mL and dumpedinto (MK2q) (clear very light yellow, pH ~13, ~220 mL). Some bubbling at the end of the dump. In a few seconds became milky with some lumps of ppt. Resuspended by mixing. Result is white ppt +clear white liq. Checking (MK20) + (MK11): dried to white crystalline crust, (MK311). Added EtOH 99%. Drying (MZ11) in warm petri. ---------------------------------------------------------------------- 2019-11-17 Sun [1] Checking (MZ11): dried to white crystalline solid with faint ocher splotches. Decanted the supernat ethanol of (MK311) into (MZ11), added more EtOH 99%. Result is milky light yellow-ocher suspension + light yellow ocher crystals. Decanted the supernat ethanol of (MZ11). Wash 3 times with EtOH 99% and some ethanol from distillation (ME300h). ---------------------------------------------------------------------- 2019-11-17 Sun [2] Washed ppt (MZ12) (olive-black) on filter paper with ~10 mL (NAH1). Dissolved into a smokyolve-black liq (MZ14) that went through the filter paper, leaving behind a small amt of yellowish-white ppt. The filtrate (MZ14) became slowly lighter until it turned clear tangerine with a small amt of ppt as grains ~0.2 mm diam. Filtered (MZ26) to remove a few bits and fibers of paper. Added to it 54 mL of Na2CO3 sol (sat at 16 C). Lilac ppt formed. Filtering (MK2q): * liq (MK312) very very light yellow clear, pH ~13 * ppt (MK313) massive snow white. Checking (MK26): lilac fluffy ppt + clear light lilac liq. Adding more Na2CO3 did not cause any more ppt nor bubbling. What is going on? What soluble complex could that be? Drying (MK312) on warm petri. Merged (ME501) into (NA0) (misc solid sodium salts with impurities). Calcinated some ppts (small amts) in a stainless steel crucible with a MAPP blowtorch, then added ~1 mL HCl 20% to each: * (MZ8): practically no residue. Discarded. * (MZ12): medium gray ash. Acid caused violent bubbling and H2S smell. Settled to black ppt +clear white liq. * (MZ5): darker gray ash. Acid had no bubbling. Result was black ppt and clear white liq. * (MZ10): almost black ash. Acid resulted in black ppt + greenish-yellow clear liq. Decanted the clear supernat of (MZ11a) to (MZ11b). Left ~1 g of light bege dusty ppt. Discarded. ---------------------------------------------------------------------- 2018-10-06 Sat [2] Filtering (MK5') (*3) using the same paper as the filtering of (MK1): * liq: clear pink, added to (MK5''). * ppt (MK10): gray fine sandy; discarded. Pipeted out the supernat of [MK7a] (~1.5 mL, clear lavender), added to filter of (MK5'). Added ~1.5mL H2O to [MK7a] (orangish-tan suspension, ~4 mL). Adding 0.21 g of (H1) to 10 g of (MK5''): formed blue ppt. Filtered the result: * liq (MK11): clear white. * ppt (MK12): blue, turned green then olive. The total (MK5'') is ~720 g, est 14.0 g (?) Added (H1) to (MK5) and (MK5'') until the supernat is clear. The ppt was blue at first, changed to pink, then to darkish turquoise green. ---------------------------------------------------------------------- 2018-10-07 Sun [1] Checking (MK5''): slightly greenish blue at pH 9.5--10. Checking (MK5): greenish blue at pH 6, supernat still light pink clear. Vacuum filtering (MK5''): * liq (MK13)+(MK13'): clear white. The (MK13) fraction went into a dirty erlen with some cobalt residue, resulting in a small amt of brown ppt. * ppt (MK14): bray-blue. Merged into (MK12). The gas from the pump of filtration (*3) was apparently corrosive. Bubbling it through a solution of Na2CO3 (MK16) turned it yellow clear sly milky. The ppt of (MK5) was bluish green at pH 6.0--6.5. Adding more (H1) turned it royal blue, with small specks white (pink?). However it turns green then olive on contact with the air. Resuspended (MK14) in H2O. Dark greenish gray susp. Filtering (MK5): * liq (MK13''): clear white. * ppt (MK14''): blue paste with olive brown surface. Washed (MK13'') with H2O; wash is (MK15). Testing (MK14) (moss green suspension): Test tube [MK14a]: ~1 mL (MK14) + 2 mL glucose sol: still gray-green at first. Test tube [MK14b]: ~1 mL (MK14) + 2 mL NaAsc sol: turned gray-blue. ----------------------------------------------------------------------