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The Silver Prospector | ||||||||
| WHERE INFORMATION AND PROSPECTORS UNITE | T | ||||||||
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Fusions to blend the following metal combinations were made on plaster tablets to avoid introducing contaminates, and to see if Tellurium can be found using microchems with only 3 precipitating reagents. It is also hoped that these microchems will detect all the elements listed. 1. Te, The primary reason for using plaster tablets to melt the various metals upon is to avoid unwanted and/or unknown contaminations that other surfaces might introduce. Plus, these white tablets are cheap to make, clean, easily handled and cool quickly. Another reason for these tests is to help determine the probability that some unknown minerals being examined are contaminated within a matrix that may include tellurium with one or more of the mentioned metals/minerals. Antimony sulphide was used in these tests instead of pure antimony metal to help introduce sulphur into these other metals that were fused together. Elemental sulphur was also combined with Te to see if a TeS could be generated by simple fusion. There are hundreds to thousands of possible combinations that can be made. Trouble is that conducting such tests is a time consuming study. The typical fire assays will not obtain this kind of information. One can spend several thousands of dollars utilizing any number of instruments to get some idea of what may be present in rock of interest. But, because of limited financial resources this type of comparison study is a good alternative which allows duplication.
10x – Tellurium melted on plaster tablet.
50x – A magnified view of the preceding image.
50x – The Te is in a solution of 1 drop nitric acid and 2 drops distilled water that has become supersaturated after about ½ hour.
50x – The saturated solution, almost dry covers the whole area of solution with this white flock that is resting on glass slide.
50x – The Te in act of digestion in Aqua Regia solution. 50x – Toothpick tip that was ignited leaving only a white residue, which would not reduce to metal no matter how many times ignited in the oxidizing or reducing part of cigarette lighter flame.
10x – The dried Aqua-Regia (A-R) solution illustrating the Tellurium that was in suspension and is now a dry white mass that has a slight/faint amount of yellow color.
40x – After driving off the nitrates from the A-R solution a couple small crystals of KI was placed in the solution. There was this immediate black precipitate, which can only be one of two items – either reduced iodine or Te. K2Cr2O7 (Potassium dichromate) and NaCl (table salt with any Iodine) do not cause a precipitation under this condition. 2… Pb + Te
10x – The fused Pb and Te on plaster tablet.
20x – A piece of the fused Pb & Te.
20x – The PbTe metal bead in a solution of 1 drop nitric drop and 2 water drops with a little heat applied to underside of glass slide.
50x – In the supersaturated PbTe nitric acid solution these white transparent to translucent crystals have formed around the perimeter of solution.
50x – Placed 3 NaCl in the Pb + Te nitric acid solution, which immediately formed the precipitate surrounding the sodium chloride crystals.
50x – A single crystal of potassium dichromate (K2Cr2O7) added to the solution slowly produced this contaminated lead chromate precipitant, which is best viewed growing on edge of chromate crystal.
50x – This tooth pick was dipped into the solution of PbTe and nitric acid prior to any precipitating reagents and was then ignited. Some small metal beads formed (likely, but not sure if a combination of Lead & Tellurium). 3… Pb + SbS + Bi +Te
10x – Image is illustrating these 4 metals fused on a plaster tablet. This photomicrograph illustrates that these metals do not like each other well enough to form a bead of obvious metal. Sme of this metal bead was digested in 1 drop of nitric acid and drops of water, which after several minutes a single crystal of NaCl was placed in the solution. Although there was a Chloride precipitate, no obvious PbCl formed. Also added a KI crystal in another part of this solution, which produced a red-brown precipitant that is in part PbI, but the red-brown is an unknown and might be an Iodide salt of Bi..This reddish-brown color may also be due too much HNO3 and not enough dilution causing the KI to partially reduce to Iodine. More tests are needed. Examine #4 for better details. Because the nitric acid digestion was essentially not a good showing, the same metal was thoroughly rinsed in water and rinsed again in concentrated HCl then placed on another glass slide to which was added 3 drops HCl & 1 drop HNO3 to create Aqua-Regia. Then it was heated to boiling till dry. Then this dry area was exposed to 2 more drops of concentrated HCl and boiled dry again and this same procedure was repeated 2 more times to eliminate any nitrates and create only chlorides.
10x – After the 4th time of driving away any nitrates a single drop of concentrated HCl was placed on slide in the dry area and a couple small KI crystals were added to the HCl solution. Immediately there was a dense black precipitant as this image depicts. The next image illustrates what happens after 20 minutes:
10x – The KI precipitated the black as the above image demonstrates, but after 20 minutes different black crystal forms began to appear, as well as the slightly yellow band in-between the two black areas. To another portion of this solution was added a single crystal of potassium dichromate, which produced no precipitant. Placed a toothpick in the original A-R before reagent chemicals were introduced, but there was no metal reduction on the toothpick. The only important aspect noticed during the toothpick fusion was an unpleasant strange odor that I cannot quite place where I have smelt it previously. Of interest is that the fusion (combining these metals) on plaster tablet produced the typical accumulation of bladed crystals in the areas that were shelted from the torch flame. Plus, much too my pleasure there are also the stacked cubic (Bi?) structures. But, oddly the remaining SbS fusions did not have the typical bladed or cubic stacked crystals as shown in next image.
70x – This is an image of what I call bladed black crystals that have a decidedly a blue tint. This portion of data is only added to represent the occassional frustrations that are part of these types of chemical tests. Note: many other reagents can and should be utilized to confirm or deny the presence of any metal. However, for the present set of images and supplementary text only the simple straight forward reagents (KI, K2Cr2O7, NaCl) are utilized. 4… Pb + SbS + Bi +Te + Ag This test with a small high purity silver prill was also alloyed with 2 additional grams of Pb, which were all re-melted together in a boneash cupel and then cupelled. The cupellation took far longer than normal suggesting that the impurities were causing cupellation problems. The following image shows the end result of the Pb+SbS+Bi+Te+Ag in cupel
20x – The end result of what would normally be considered a botched cupellation.. Obviously this is a mess with all the semi-metallic looking blacks and orange grunge which partially hiding the metal bead at about the 2 o’clock position.
40x – A closer view of the black semi-metallics, which may be a form of Te, as well an accumulation of metal spheres near center of image.
40x – A much better view of the obviously contaminated silver that is blackish grayl. In fact this would normally be considered a disaster and not worth pursuing. However, I don’t throw away these undesirable assays, because all mistakes or errors are lessons to be learned. So, I do what others won’t – I keep digging trying to get a better idea about the why’s and what went wrong. The black looking metal was removed and surface etched in nitric acid and water as good as possible. Then this blackish bead placed on another piece of bonash and cupelled.
40x – Even this 2nd cupellation ended in another mess. Obviously the silver is so contaminated with Te and possibly other original metals that grunge is piled all over the silver bead that can be seen with this magnification, but not with the eye.
50x – Retrieved the silver prill from the cupel and tried to slowly use diluted HNO3 acid to strip away as much of the grunge as possible.
50x – The contaminated silver prill is almost free of the adhering grunge.
50x – The blacks are laying on slide, but eventually dissolved.
50x – After the prill was digested the nitric acid/water solution was becoming super saturated causing this crystal formation to precipitate along the perimeter of solution. This is obviously not a pure silver solution precipitant.
50x – As the solution continues drying this perimeter of saturated nitric acid the structure of the saturated nitrates change.
50x – The solution becoming more dry naturally.
50x – The solution became dry, so one drop of water was added to solution area and a single K2Cr2O7 crystal was placed in the now diluted solution residing upon glass slide. Although red colored blades are growing on this crystal of potassium dichromate they are not classic pure silver.
50x – This image attempts to show how Pb chromates are flowing away from the potassium dichromate crystal.
50x – As the diluted solution nears dry these red crystals have formed and are not indicative of silver chromate, although silver is likely present.
50x – In a companion test solution pipetted ( I often slaughter the English language with my own created words) from the diluted solution a single crystal of NaCl (table salt without any Iodine) was introduced, which produced an immediate typical AgCl (the large white semi-circular area) precipitate.
50x – Placed a toothpick tip in the solution prior to any additions of reagents that would cause precipitants, so that only what is in the solution might be reduced to metal when the metal laden acid impregnated the wood fibers when the oxidizing or reducing parts of a cigarette lighter flame ignited the toothpick tip. 5… Pb + SbS + Te
10x – The Lead, Antimony sulphide (stibnite) and Tellurium fused into a single mass on plaster tablet. This metal blob does not resemble shinny metal, but was somewhat shinny when in a molten state.
20x – The above pictured metal was placed the solution of 1 drop nitric acid and 2 drops water, with a little heat to promote the digestive action.
10x – Another sample of Pb+SbS+Te conducted at a later date, basically showing same result as the above image, but the colors are more accurate here due different microscope and lighting. Again, the probability is that the white mass is Sb. Ran a toothpick check and metal balls formed, but were too small to get a decent image of.
50x – This image shows the gel-like white (Sb?) crystals, as well as transparent crystals which appears to be Lead Nitrate.
50x – To confirm the presence of the metals in solution a couple small K2Cr2O7 crystals were placed in the solution. It did not take long for an grange and yellow precipitant to form. The yellow crystals not easily seen here are likely Pb, however the yellow crystals became totally captured by the orange precipitant.
50x – The potassium dichromate has become partially decrepitated.
70x – The magnified previous image. 50x – A single sodium chloride (NaCl or table salt without any Iodine) placed in a different position but unaffected area within same solution as shown in preceding image. This salt crystal immediately began forming the traditional PbCl crystal growth. But, these crystals do not show any inclination to form the normal Pb feathers which suggests interfering contamination, which may be due to the Te and/or Sb.
50x – Added a single crystal of KI (potassium Iodide) to same solution as mentioned above, but in a isolated area unaffected by the other additions. Prior to adding the KI two drops of water was added to significantly dilute this portion of solution. The image has captured a yellow band of precipitants at left of center and is typical of Lead Iodide.
10x – The exact same test as immediately above (1 drop HNO3 + 2 drops of distilled H2O), but ran at a different date and further diluted by 3 additional drops of water for a total of 7 drops of water, which immediately produced when adding 2 small KI crystals the classic yellow Lead Iodide precipitation. This demonstrates that good results can be achieved with KI in nitric solutions, but for me a lot of trial and error is required. The next image is of the same area as shown here, but magnified to better illustrate the white to gray precipitate laying close by and all over the bottom of solution.
40x – This image shows a bunch of whitish-gray precipitated crystals close to the Lead Iodide crystals that resemble gelatinous silica, but is not silica.
50x – The original PbSbSTe metal blob used in the above prior test solutions was now rinsed in distilled water then rinsed in concentrated HCl to strip away any nitric acid. Then this metal bead was placed on another clean slide and submerged in concentrated HCl and heated. The heat generated with this HCl eventually caused these crystals to form on the perimeter of solution as a result of drying and super-saturation. Although I did not smell the odor of sulfur in the nitric acid digestion I sure was aware of the sulfurous odor with concentrated HCl when heated, which liberated to liberate these copious vapors. Although I avoid breathing fumes from fusions or these microchems it is often unavoidable and I find significant data with these odors, which are quite varied and not likely to be noticed any other way.
50x – more of the super saturated crystals in same concentrated HCl solution.
50x – When a KI crystal was first added to the HCl solution no precipitant formed except for a pretty yellow color of solution surrounding the KI crystal. Then the KI began causing some precipitation and solution colors especially along solution perimeter where the clear saturated crystals had formed in the previous image. .
50x—In same HCl solution these radiating white to clear crystals formed next to the metal bead as a result of the KI, which I suspect is a form or Pb. Plus, there are also red precipitants forming at right of the white crystals that the KI apparently is causing. Don’t know what these tiny red crystals are. By accumulating a battery of images using various acidic mediums and a variety of chemical precipitants considerable clarification can be accomplished as to what a mineral is or not. Ran a toothpick test on the HCl solution, but it failed to reveal any metal.
40x – This image is of a A-R solution that was converted to a chloride state with 4 evaporations using concentrated HCl, to which 3 small KI crystals were added, which produced this group of blacks. The reason that 3 KI crystals were added instead of 1 is a result that when I used a wetted tip of toothpick to grab hold of the KI instead of what my eye saw there were actually 3 tiny KI particles.
10x – This is the same image as above, but at a reduced magnification. By the time I was able to capture this image the KI crystals of the above image had dissolved. It appears that this black formation made-up of zillions of tiny crystals is one of the forms of TeI and not a KI reaction with residual HNO3, 6… Ag + Te
35x – The Ag+Te fused together on plaster tablet. The area at about 6 o’clock on this metal bead has a slightly raised pearly looking surface and the rest of prill is essentially blackish-gray with a metallic appearance..
20x – The AgTe in solution in the act of being digested in 1 drop HNO3 & 3 drops H2O.
50x – The AgTe prill digesting in 1 HNO3 and 3 H2O, creating piles of shinny metallic looking black crystals accumulating on the glass slide.
50x – Some AgTe crystals due to super-saturation are forming along perimeter of solution.
50x – The AgTe in a saturated solution produced these forms of crystals, which is clearly not Silver, but may be a combination of both elements.
70x – More of the super-saturated Ag+Te crystals within the boundaries of the larger white crystals I do not know what these crystals are, but are apparently some kind of nitrate combination.
50x – To the same HNO3 + Ag+Te solution was added 2 crystals of NaCl, which instantly formed the typical silver chloride precipitant that keeps expanding till all the NaCl is consumed or the amount of silver nitrate in solution becomes AgCl. If this AgCl is left to sit for several minutes to a few hours the bluish rose-purple color will form, eventually becoming black because AgCl is light sensitive as seen in the next image.
50x – As the preceding solution continues drying and the light within the room shines on the AgCl precipitant it is slowly turning lavender along the edges.
50x – The Ag+Te nitric acid solution with a single introduced crystal of potassium dichromate is forming what appears to be a typical silver chromate precipitant growth of red crystals. However, although one would say that silver is present these red crystals are a little different than what a pure silver solution would produce. So, apparently the Te is influencing these red crystal growths.
70x – A magnified view of a portion of the red (Ag+Te) crystals in the above image.
50x – A toothpick tip is dipped into the Ag+Te + HNO3 + H2O solution This wood tip is exposed to the tip (oxidizing or highest heat source) of cigarette lighter flame, which produces (reduces) a series of wire looking metal strands and a few larger metal beads. It took 2 relatively short exposures to the flame for this metal format to show good enough to be photographed. Often, metal formed in this manner can be further consolidated into a large metal bead with more exposures to hot flames. 7… Te + S
10x – Te + Sulphur fused on plaster tablet. The hope was to obtain tellurium that chemically combined with the sulphur to form a sulfide or something close which I could eventually identify with acids and chemicals.
20x – From the above plaster a piece of the semi-brittle Te+S fragment on a slide with 1 drop nitric acid and 2 drops water and heated. When dry and 2 drops of water was added the white precipitant does not dissolve, but when HNO3 is added the white mass it readily goes back into solution. The addition of a Potassium dichromate crystal only produces a red solution and no precipitant.
20x – Forcing the solution containing the potassium dichromate crystal to dry continues to produce a deep red coloration, which is almost black, but nearby the previous white is turning a pretty light sea green. The greenish color may only be a liberated chromium salt.
20x – After rinsing in water, followed with a concentrated HCl rinse to expel any trace of nitric acid the same Te+S fragment is placed on another glass slide. These types of bands should not be construed as positive proof of anything, but might be a clue for future tests. Even though a couple of these tests proved that adding acid or water to concentrated solutions can and will either digest or precipitate one or more of the elements, no attempt was made to determine nor carefully manipulate pH levels. I prefer to always start microchems using concentrated acids and as few precipitating reagent chemicals as possible. In other words I try to keep it simple, if possible. Finally, although finality is a long way off, it's crystal clear that other reagents are necessary to prove when and if Te is present when numerous other potentially interfering elements are known or likely to be present in any of the solutions. |
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