Sei sulla pagina 1di 23

How to Find Gold California Gold Rush History (18481855) instigated on January 1848, when gold was discovered

at Sutters Mill. James Marshalls discovery of a nugget that was the size of a dime in the tailrace of Sutters Mill started this frenzy. A man named Sam Brannan was the one that announced that gold had been found in the American River and showed a bottle full of gold nuggets. James Marshall found a gold nugget that had the size of a dime in the tailrace of Sutters Mill. Sam Brannan was an elder in the Mormon Church and he had a general store in Sutterville, which was a small town on the Sacramento River. Since Sam knew that gold seekers were going to start going into Sutterville, he placed a stock of shovels, picks and a lot of other mining equipment prospectors would need in his store because he knew that these people were going to have to pass by his store before going out to get the gold. The next thing Sam Brannan did was go through the town and fill every one on the wonderful news and started a booming business from one day to the next; he obviously got rich due to this well thought up plan. John Sutters story was totally different though. He travelled to America in 1834 and left his wife and children behind in Germany. His original name was actually Johann August Sutter but he wanted a name that sounded a bit more American so he changed it to John Sutter. He turned into a trader on the Santa Fe Trail and had been told stories about the rich land that was in the west in California and had been told a man could own as much land as he desired. When he found out about this he decided to leave his trading post and set out to California and became a rancher in 1838. It took him about a year before he actually got to California. In 1839, July 5 the govenor of California who was Mexican gave John Sutter permission to choose a tract of land located on the east of the San Francisco Bay to settle down in.

By 1841, Sutter became a Mexican citizen and was given 49,000 acres of land. He decided to settle in an area where the American and Sacramento Rivers joined. He decided to build his fort on a hill that over looked the rivers. His fort was eighteen feet high, the walls were three feet thick and he placed cannons on the corners. The fort he had built was similar to a little city and had a tannery, distillery, gristmill, blacksmith, carpentry and a blanket weaving shop. The only thing that Sutter did not have was lumber. However there were a great amount of trees in the mountains to the east, so he decided to build a saw mill on the American River on a site that was called Coloma so that he could get lumber for

the fort. James Marshall was a carpenter that worked for Sutter and Sutter asked Marshall to build and operate the mill and that if this were done they would divide the profits. On the 24 of January, John Marshall made the discovery that ended up changing the history of America. Marshall had directed the water from the millpond into the tailrace so that it could get washed and cleaned from the dirt it had on it. The next morning when he was checking the tailrace to see if it was clean, he noticed there were a lot of little pieces of bright yellow metal shining. He picked up these shiny pieces of yellow metal and studied it a bit. Then he decided to test it to see if indeed it was by pounding on the metal with a hard rock; when he saw the metal flattened out with no trouble, he knew it was gold. Process Flowsheets of Gold Plants

Safety Equipment to Fire Assay: Personnel Protection

Eye protection, gloves and coveralls should be worn at all times. Hygiene should a top priority for everyone.

The equipment such as the loading forks, pouring tongs should be supplied as one is dealing with extremely high temperatures.

Fire Assay Terms and Terminology


Here are some word or talk/terms of the trade we using in assaying: Annealing the heating of gold after parting to change its colour from black to gold. Bead Particle of gold and silver that is obtained at the end of the cupellation process. Borax An acid flux. Crucible A bone ash vessel in which the sample and fluxes are melted. Cupel A shallow cup which the lead button is oxidized during cupellation. Cupellation Process of burning off the lead button. Feathers crystals of lead oxide on the edge of the cupel. Indicates that the cupellation worked as it should. Flux reagent mixed with a sample that aids in the fusion process. Freezing of the cupel - A condition in which solid lead oxide or other solids cover the surface of the molten lead in a cupel. Fusion Process of heating a charge in a crucible to cause reactions and produce a

molten liquid. Inquartation The addition of silver to ensure that the bead will part. Lead button - Metallic lead produced during a fusion and becomes solid in the mould. Lime - A basic flux. Litharge Lead oxide, a basic flux and a source of lead used in fire assay. Microbalance A very sensitive balance that weighs beads. Mould An iron cone shaped vessel, which fused materials are poured into. Muffle A chamber in a furnace in which fusion and cupellation are carried out. Opening of the cupel - At the beginning of cupellation when the surface of the lead oxide melts. Ore A natural material that came from the earth, that is to be assayed. Oxidizing agent An ore or a reagent that supplies oxygen for reactions during the fusion. Parting Method of separating gold and silver by dissolving the silver. Parting acid - Nitric, Hydrochloric and Sulphuric acids. Parting cup - A porcelain vessel which parting, rinsing and annealing of the gold takes place. Reducing agent An ore or reagent that accepts oxygen during the fusion which helps in the formation of the metallic lead. Reducing Power The ratio of lead reduced during the fusion to the weight of the reducing agent added. Scorification An oxidizing fusion of a sample with lead and borax in a shallow dish. Slag A fused mixture of non-metallic sample ingredients and fluxes, usually contains silicates. Soda ash - Sodium carbonate, which is a basic flux. Oxidizing Fluxing Reagents used in Fire Assay The oxidizing power in fire assay is the ability of a substance to give up its oxygen. Nitre (potassium nitrate KNO3): Nitre is an important and powerful oxidizing agent. It oxides sulphur and many metals by releasing its oxygen. For example it is used quite regularly in the assaying of zinc, lead and copper. It oxidizes sulphides to sulphates, arsenides to arsenates and most metals to their oxides. It is used mainly in high sulphides samples to control the size of the button. If large amounts of nitre are needed to fuse a sample one must pay attention to the temperature of the charge to prevent boil-overs. One should try to heat the charge in evenly and gradually. Nitre is also known as desulphurizing agent. In the process of fusion, it decomposes in 2 stages. The first stage is to KNO2 and then to K2O at a higher

temperature: 2KNO3 = 2KNO2 + O2 2KNO2 = K2O + 2NO + O Red Lead (lead oxide PbO:Pb2O3 or Pb3O4) can be used for its oxidation action in a fusion and it is used to replace litharge. It is used in a limited way because it can produce too much lead in the fusion mixture. The oxidizing power of red lead comes from the release of O2 when it is heated. The PbO that is produced is further reduced to Pb by sulphides in the sample. Hot air is also an oxidizing agent. The oxygen that is in the air is the oxidizing agent, which is similar to red lead. Reducing Fluxing Reagents for Fire Assay Reducing samples are ores that contain sulphides, arsenides and carbonaceous substances. One wants to reduce the litharge to lead, PbO Pb. The reducing power is the amount of lead that one gram of an ore or reducing agent will reduce. Flour is the most commonly used reducing agent. It is used in samples that have little or no sulphites in order to reduce the litharge to molten lead for the collection of gold and silver. Carbon is the active ingredient in flour. The flour that used is ordinary wheat flour. It is has several advantages. It is cheap and it is readily available. It also is very fine and mixes well with the ores and fluxes. One thing that one should consider when using flour is that flour has varying moisture content. Generally, 1 gram of flour will reduce 11 grams of Pb. Tartar (potassium bitartrate KHC4H4O6): This is cream of tartar or potassium bitartrate. The carbon and CO act as the reducing agents. It has less than half of a reducing power then flour, about 2.5 grams is required to reduce 11 grams of Pb. Charcoal is about 90% carbon. It has been used in the past but it is not as common now. It reacts with metal oxides by the production of CO2 at lower temperatures and CO at higher temperatures. It has twice the reducing power as flour, but the quality can vary. List of Neutral Fluxes and Neutral Sample: Fire Assay Neutral samples are ores that do not reduce or oxidize and are neither acidic nor basic. These ores are fluxed with a standard premixed flux. Neutral fluxes are used mainly to help control the fluidity of thick slag.

Fluorspar (calcium fluoride CaF2): It is used as a flux in fire assaying because it increases the fluidity and helps with difficult pours. It melts at a high temperature and is very fluid. It suspends the infusible particles without lowering the fluidity of the slag. It is mainly used in fluxing ores containing calcium phosphate (bone ash), barites, gypsum, and infusible silicates. Fluorspar melts and remains unchanged in the slag. Fluorspar gives a stony appearance to the slag. Salt (sodium chloride NaCl): Slat is added as a cover to fusions to protect the flux from air oxidation. It is very fluid and it is used to wash down particles of the metal that stick to the sides of the crucible. It is unchanged during the fusion. Cryolite (AlNa3F6): Cryolite is used as a flux to aid in the fluxing of high Al2O3 ores such as clays and occasionally in the melting of bullion. List of Acidic Fluxes used in Fire Assay Acid Fluxes: Basic sample require an acidic flux to produce an ideal slag. An example of a basic sample would be limestone/dolomite samples. One can performed a quick test to ensure that a sample is limestone by adding a couple drops of HCl acid. The samples will fizzes which is the CO2 that is produced. Borax Glass (sodium tetraborate Na2B4O7): Borax glass is a strong acid flux and it is used in almost all fusions. Borax glass can act as an acid and base. Borax has several helpful properties in the fusion process. It lowers the fusion temperature for the formation of slags. It is capable of fluxing most metal oxides. It also increases the fluidity of the slag, which can help with difficult pours. The addition of too much borax can result in a very tough slag that is hard to separate from the button. The slag sticks to the button and results in a loss of precious metals and low results. One also should decrease the amount of borax when dealing with a high grade copper sample because the bead can be absorbed in the cupel during the cupellation. If one can not decrease the amount of borax in a flux to resolve the problem, one can add a basic flux which can provide a solution to the problem. Hydrated borax (Na2B4O7 * 10H2O) it should be avoid because it often produces boil-overs because the salt in the borax loses water and causes swelling of the charge during the fusion. Silica (SiO2): Silica is the strongest acidic fluxing reagent. It combines with the metal oxides to form silicates. The silicates are the foundation of all slags. It is a

fine powder and is added to samples which are basic to help protect the crucible in the fusion process. When too much of silica is in the flux, it can reduce recovery of the precious metals because of the precious metals that can be lost in to the slag or the formation of matte. Powdered glass can be used as a substitute. The amount of SiO2 varies in glass and therefore may cause a problem with an assayer ability to perform reproducible assays.

List of Basic Alkaline Fluxes used in Fire Assay Sodium carbonate (Na2CO3) or Soda ash: Sodium carbonate is a powerful basic flux that reacts with silica-based (acidic) minerals to form a fusible sodium silicate. Na2CO3 + SiO2 = Na2SiO3 + CO2. There can be problems with soda ash reactions. The CO2 gas that is produced can cause frothing if the temperature is too high. Soda ash is very fluid and can hold finely powdered materials such as carbon (flour) in suspension in the melt which can interfere with the formation of the button in the fusion process. Soda ash can also act as a desulphurizing and oxidizing agent. Soda ash is also very corrosive towards the crucible. Sodium bicarbonate (NaHCO3) baking soda: This can be used in place of soda ash but it is less common. It has less soda, which is the active ingredient. It loses water and CO2 at low temperatures and can cause losses due to, cross contamination, frothing, and the sample boiling over. The end product of the use of sodium bicarbonate is the same as with soda. Litharge (lead oxide PbO) & Red lead (lead oxide PbO:Pb2O3 or Pb3O4): Litharge (PbO) or red Lead (Pb3O4) is a basic flux that has many purposes. It helps to decompose silica to form fusible lead silicate. PbO + SiO2 = PbSiO3 It supplies the lead to produce the lead button that collects the gold and silver. PbO: 2PbO + C(flour) = 2Pb + CO2. It also dissolves difficult-to-fuse metal oxides for example Copper. One should practice some caution because excessive litharge corrodes the crucible and destroys the furnace floor if there is a spill or boil over. Red lead acts as an oxidizing agent as it decomposes to PbO and gaseous O2 on heating as oppose to CO2 and is sometimes preferred to litharge. 2Pb3O4 = 6PbO + O2.

Hematite (iron oxide Fe2O3): Hematite is sometimes used as to replace litharge. It is combination of a basic flux and an oxidizing reagent. Ferric oxide is very difficult to fuse but is reduced to a more easily fused ferrous state during the fusion. It then combines with silica to yield ferrous silicate. Manganese oxides act similarly to iron oxides. These oxides act as oxidizing agents by consuming carbon (flour). 2 Fe2O3 + C = 4FeO + CO2 2 FeO + SiO2 = 2FeOSiO2 Lime (CaO): Lime also known as the mineral limestone (CaCO3). It is a powerful base for fluxing the silica. On heating, limestone loses CO2 and reacts with silica and produces a fusible silicate. Calcium also is found with magnesium in a carbonate mineral called dolomite (CaMg(CO3)2). Magnesium behaves very similarly to calcium in a fusion. Desulfurizing Reagents In fire assay, desulphurizing reagents are substances can attract sulphur and pull the sulphur away from the other compounds.

How Is Gold Purified? 1. Gold is purified through a process of high temperature heating or chemical exposure, depending on the purity of the mined gold, according to ResponsibleGold.org. Initial Processing of DifferentTyes of Ore 2. If the gold is a low grade ore, then it is broken up into chunks that are then put in carefully lined pads and treated with a dilute cyanide solution, which dissolves the gold. For high grade ore, the metal is sent to a grinding mill and made into a powder. Refractory ore contains carbon and is heated to over 1000 degrees F, which removes sulfide and carbon. The resulting oxide ore is directed to the leaching circuit. Sulfide refractory ore that contains no carbon is oxidized in an autoclave to free gold from sulfide minerals, then it is sent to the leaching circuit. Further Refining 3. At this point, treated high grade ore is leached with cyanide and gold is collected onto activated carbon with the cyanide solution being recycled. The gold-carbon mixture is put in a vessel where the gold is removed chemically. The carbon is then recycled. The gold is then extracted from the solution by electrolysis or chemical substitution. Purifying the Gold

4. At this point, the gold is melted into dore bars composed of 90 percent gold. The bars are then sent to an external refinery to make them 999.9 parts per thousand pure gold. Other Means of Refining Gold 5. According to Hoover and Strong, a refiner and manufacturer of precious metals, they produce 98 percent pure gold using the Miller process. After a sample of treated impure gold has been tested in a lab for purity, the gold is melted in a furnace, then chlorine is bubbled through the liquid. The chlorine attaches to elements in the gold that then become solid and move toward the top of the furnace. They are skimmed off. Electrolysis is ultimately used to purify the gold

How to Purify Gold Gold Melting Before gold is sold on the market it has to go through a purification process. This process is quite complex and dangerous. It needs to be done under the right circumstances and with the utmost care in safety precautions. It is not recommended to try this process unless you have experience working with harmful chemicals. Difficulty: Challenging Instructions Things You'll Need:

2 beakers Hot plate Glass rod Coffee filter Gold ore Hydrochloric acid Formic acid Nitric acid Sodium sulfite Uniodized salt Borax 1. Step1

Prepare your beakers. Place your gold ore into one of the beakers. In your second beaker, mix three parts hydrochloric acid to one part nitric acid. Be very careful when mixing your acids, as both are quite toxic and can be dangerous. Be sure that you are also wearing protective eye wear as well as gloves that can hold up against acid. 2. Step2

Mix your acid beaker with your ore beaker and simmer. Be careful to do this quite slowly and carefully. Once you have combined your two beakers, simmer the mixture on a hot plate until all of the nitric acid has been boiled off. If most of the liquid evaporates before the nitric acid is gone, you can add a small amount of hydrochloric acid to keep the ore covered in liquid. 3. Step3 Filter the solution. Use a strainer to filter off any of the solid that may be left from the boiling process. Do not dispose of the solid without first treating it with a solution, such as lime juice, to neutralize it. After you have strained out the solid, add equal amounts of distilled water, as there is liquid in the beaker. 4. Step4 Check for silver. Before you can extract the gold, you must first extract any silver that may be present in the ore. Slowly drop small amounts of the uniodized salt into the mixture. This should cause little white particles of silver chloride to drop to the bottom of the container. You can then use a coffee filter to strain out the liquid from the silver particles. Set the silver aside. Be sure to keep the liquid that you have strained off because it still will contain the gold. 5. Step5 Check for gold. Put the remaining acid mixture back into a beaker. Slowly add sodium sulfite to the mixture. This will cause the gold to continue to add the sodium until the gold stops moving to the bottom of the beaker. Filter the solution again using a coffee filter. Rinse and dry the filter containing your gold. 6. Step6 Heat the gold. Now that you have your separated gold, put the filter into a clay crucible, and set the filter on fire to get rid of it. Cover the gold and the filter with borax, and place in a furnace that is capable of reaching temperatures of 2,000 degrees F until the gold is smooth. Pour into a mold and let it cool.

How to Start a Gold Refining Business You can make money starting a gold refining business if you get the right tools, supplies and chemicals. The demand for scrap jewelry is rising and becoming very popular among gold producers. Simply put, gold refining separates and purifies the gold from other metals. The dental and electronics industry frequently use refined gold products. So basically, you will be preparing gold to be used in various industries. Difficulty: Challenging Instructions Things You'll Need:

Simplicity gold and platinum refining system Electric gold and platinum tester

Battery charger Electric melting furnance Crucibles stirring rods and flux Ingot mold and gloves Step1

Make sure you have the financial capital to start a gold refining business. If you do, visit the Small Business Administration (SBA) website at sba.gov. Answer all of the questions under the Small Business Readiness Assessment Tools section. This tool will help you discover your weaknesses and strengths before you start your gold refining business.

Step2

Search in your area to find a gold refining business and try to work there for free until you learn the business. Interview the owner by phone or in person and ask him how he started his gold refining business.

Step3

Once you have developed the skills needed to start your gold refining business, decide what type of gold refining business you want to start. In this example, you will be able to work at home, in an office, or out in the field. Call (914) 667-1100 and ask for the customer service department. Inform the service representative

that you want to order a gold refining kit to start your gold refining business. Step4 Service representative will inform you about what items you will need to purchase to get started. Make sure that you also inquire about discounts and other products that may be available at no cost. After you have paid for the products and have received them, take a trip to your local office supply store and buy all the office products you will need (i.e., business cards

, invoice forms, copy paper).

Step5

Your business plan should explain how you will get customers (i.e., jewelry repair depts., jewelry manufacturers' etc.). Include how you plan to operate each day. Set up a financial plan to monitor your cash flows. Go to your local city or county office and apply for a permit or license to operate your business. Apply for your state tax ID number at govspot.com. Find your state and apply online. Call (800) 829-4933 and apply for your federal tax refining business started. ID number. These steps will help you get your gold

Gold Smelting and Refining Gold concentrates: The options for treating gold concentrates are in direct relation with its gold contain, thus gravimetric concentrates have been treated by amalgamation following by retorting of the amalgam and smelting of the product.

This is usually still the most efficient option, but considering the health hazard of mercury, several alternatives must be considered. High grade concentrates, typically more than 300-500 g/t can be directly smelted, provided that the material does no contain minerals that could adversely affect smelting, e.g. sulphides. Sometimes flotation can be used to up grade concentrates for direct smelting, but this is rarely applied. The effectiveness of the process depends on the nature of the material and the degree of gold liberation. Smelting is an option for treating gold flotation concentrates, however the lowest grade that can be considered for smelting is more than 300 g/t, depending on the content of other metal values (copper, silver, platinum group metals), the concentrations of penalty elements and shipping distance

Fig. 6.1 Smelting of Dore Bullion

How to Load an Assay Furnace for Refining / Smelting


Load and place the mixed charges into a furnace between 1900 - 2000oF. As the mixture heats up, litharge is reduced to lead by the carbon or sulphides of the

charge. The sample minerals fuse and the shots of lead then take up the freed gold and silver from the surrounding particles of ore. This produces an alloy with the lead and the precious metals. At the same temperature, the borax of the charge begins to melt and forms fusible compounds with some of the bases of the flux. The fusion usually takes 45 minutes at a temperature between of 1950 to 2000 0F. Lead oxide and silica combine and from this point the slag begins to form rapidly. The slag remains vicious until the ore particles are thoroughly decomposed and every particle of gold and silver has been taken up by the suspended molten lead. The slag becomes thoroughly fluid, and the lead falls through the slag, collect at the bottom of the crucible. Samples that required a high nitre flux or gasforming substances such as carbonates, close attention should be given to the crucibles because of possibility of boil overs. If there is evidence of frothing, the door should be opened to cool the fusion down. The molten mixture is poured into a metal mould where the Pb collects beneath the slag as a small cone. Pouring moulds are conical iron depressions.

When the assayer is pouring the flux charge of molten mixture in to the mould, the assayer should pay attention to the way the mixture pours and if there is any evidence of shots of lead. This can be good indication of if there will be problems and undesirable products.

Dissolving Silver away from Gold using Parting Solutions


Parting is the process of dissolving the Ag (Silver) in the bead from the cupellation to leave the Au (Gold) behind for weighing or to be read on the AAS. If Ag is to be determined gravimetrically as well, the bead is weighed before parting. The very small beads are weighed using sensitive micro-balances.

Parting solutions: Nitric Acid (HNO3) Dissolves Ag and Pt group metals & leaves the gold behind.
Sulphuric Acid (H2SO4) dissolves Ag ; leaves the Pt group metals & gold behind. Hydrochloric acid (HCl) In the AA finish, HCl is added after the Ag is dissolved to form aqua regia (3:1 HCl to HNO3) . Aqua regia dissolves the gold Ammonia (NH4OH) used to dissolve any possible silver chloride which may have precipitated out.

Nitric acid is almost used all the time but sulphuric acid can be used as well. Nitric can not be used unless there at least three times the amount of silver than gold. The idea of parting is to prevent the gold from breaking up into small particles. The gold that remains in one piece is much easier to handle.

Acid concentrations.

Gravimetric finish 6:1 HNO3 for gravimetric finish 3:1 HNO3 for gravimetric finish 1:1 HNO3 for gravimetric finish 1:5.5 H2SO4 for gravimetric determination Of Pt Group metals.

Instrumental finish:
0.5 ml HNO3 of concentration for AA finish 1.5 ml of conc. HCl for AA Finish

Roasting of Gold or Precious Metal Samples


Roasting is a technique used to handle difficult gold or precious metal samples. Minerals decomposed in this way include sulphides, arsenides, antimonides and tellurides. A successful roasting can render samples amenable to standard flux mixes. Weigh 50 grams of a sample into a shallow dish and place it into an open furnace at 100 0C. Raise the temperature slowly to 600C with careful stirring. When no fumes are seen, raise the temperature to 700C for 20 minutes. The S, As, Sb, and Te are lost as volatile species. Their elimination simplifies the fluxing and prevents the formation of speiss or matte deposits. Care must be taken not to fuse galena because Ag is lost during thisroasting process.

Improve Precious Metals Recovery with Slag Quality


One must try to produce an ideal slag because it will help with the recovery of the precious metals. The best slags are a balance between acidic and basic properties. Slags are classified according to the proportion of oxygen in the acid to the oxygen in the base. A mono-silicate slag has equal amounts of oxygen in each whereas bi-silicate slags have twice as much oxygen in the acid as in the base. The best slags are those that range between a subsilicate and a bisilicate. The different fluxing reagents all have a role in producing an ideal slag. The fluxing and fusion procedures require that the fluxes balanced each other. It should be glassy and homogeneous in colour and texture. Streaky slags are a sign of an imperfect fusion. A sample that indicates high S, As, Sb, Cu or any other base metals requires a knowledge of how to proceed with the fluxes that is gain by experience and asking question from those assayer whose do have the experience.

Here is a list of some common slags. Various Greens = Ferrous Silicates Brick red = Copper Opaque Milky White = Ca, Mg, Al, Zn, Ba - Limestone sample will produce a greenish, opaque and/or streaked slag. Black = Fe & Mn

Blue = Co Purple to light Pink = Mn Greenish white = very high sulphide.

Fusion tips.: Place crucibles in sequence after pouring. A rack should be set aside to dispose the hot
crucibles.

Set aside crucibles with unusual pours or lead buttons. A history of difficult or problematic samples should be kept.

Lead button size.: The size of button to aim for is a range from 20 to 35 grams

Separating / Removing Slag from the Gold rich Lead Button


When the slag is cooled, the slag is separated from the Pb button by pounding it off with a hammer and then cubing the Pb button so it can be easily picked up. The lead button should be bright, it should separate from the slag easily and there should be no evidence of matte or speiss on the top surface of the button. The Pb buttons should be between 15 to 35 grams. One should keep a record of past sample fluxing history as to change and improve on the fluxing of difficult samples. This can help to attain correct button size, poor slag/ button separation, matte or speiss and other problems. After the fusion material is poured into mould and cooled, the lead button is separated from the slag by hammering the slag off the button.

There are two undesirable products matte and speiss that are occasionally obtained. There can be a third product if salt is used or if nitre is used in the assay. The third product will be found on the top of the solidified slag.

Matte is an artificial sulphide of metals found in the ore and /or flux. It is formed in the nitre fusion of sulphide ore when the charge is too acid. It is found just above the lead button. It may be quite thick, or it may appear simply as a granular coating on the upper surface of the lead button. It is usually blue- grey in colour, resembles galena and is very brittle. The matte always carries some of the gold and silver. It is usually broken off and lost in the slag during deslagging of the lead button leading to low results. If it occurs, the assay must be repeated with more basic fluxes and less acid fluxes.

Lead shot in the slag: This is usually caused by the temperature being too low or too little silica in the charge. Should shooting occur, increase the amount of silica and litharge and re-fuse at a higher temperature.

Speiss
In the fire assay speiss is usually a combination of Fe & As. Speiss is formed when the iron method is used on ores containing arsenic. It is a hard, fairly tough, tin-white substance found on the top of the lead. If a small amount of arsenic is present, the speiss will form a little button on the top of the lead. If there is lot arsenic is present, thespeiss may cover the entire top of the lead. Speiss contains Au & Ag, and may be cupelled along with the lead if there is less than a gram of speiss. Larger amounts are difficult to deal with and the sample should be assayed by another method.

Inquartation
Inquartation happens because in order for the fire assay of precious metals there needs to be a collecting agent that assists in the parting process. A small amount of silver is usually added to the crucible during the mixing of the fluxes. There has to be a ratio of 3Ag:1Au for the parting process to proceed and for the parting process to work properly. There are different ratios required for gravimetric and instrumental finishes.

Instrumental Finish in Gold Analysis


One should first pick and flatten the beads and put them into 16 x 125mm disposable glass test tube. One should ensure water bath is a minimum of 75 0C. Another option is the use of fine sand. The sand gets far hotter than a water bath.

The assayer should add .5 ml of concentrated HNO3 from a calibrated dispenser and place rack in hot water bath for 15 minutes. After 15 minutes the assayer should confirm by visually inspecting the test tubes for the complete silver digestion. After the assayer confirms that the silver bead is digested, one can proceed to digest the gold by dispensing 1.5 mL of concentrated HCl from a calibrated dispenser into the test tube. Once both the acids are added one should again inspect each of the test tube for complete digestion of the gold. The final steps are to dilute to the final volume and shake the test tube to mix the solution thoroughly. The addition of the acids should be done inside of a fume hood because of the fumes that are produced. Bead parting tips for readings done on an AAS or ICP OES/MS are as the follows. One should check that each tube has a bead in it. One should also check that the acids are dispensed correctly. The aqua regia should be an orange/yellow colour. One can look for the AgCl precipitate in each test tube. For the measurement of gold by AAS or ICP/OES measurement, the entire bead must be dissolved so the instrument can measure the solution concentration. The instruments determined the concentrations by aspiration the sample into the calibrated instrument. This instrumental method is much more common for finishing then measuring with the gravimetric technique. The instruments are capable of a much lower detection limits. Labs can measure a 1 or 2 ppb detection

limits using AAS, ICP OES and ICP MS.

Gravimetric Finish in Gold Sample Analysis Technique


Proper Gravimetric Technique starts with ensuring parting cups are clean before using. The assayer should put a flatten bend in hot 6:1 nitric to start, and watch the bead for its reactivity, add stronger acid if it is needed. This should be done on a hot plate and inside a fume hood. If stronger acid is needed it should be hot. One should carefully add and remove the acid with a disposable pipette. To make sure that floaters are fully parted, use glass rod or tap cup to sink to sink them. One can add ammonia rinse solution and to remove any AgCl that is present. There are microbalances that can go down to 0.1mircograms which allows the gravimetric detection limit to improve over the gold balances in the pasts. Handling the very small beads can be very difficult, so gravimetric finish is reserved for higher grade samples. Analysis of gold was by fire assay, with a gravimetric finish on samples exceeding 3 g / t gold

Rinsing. After parting is completed, one should rinse the bead. One can use rinse with 14:1 NH4OH to remove any residual AgCl or use distilled water.

Drying & Annealing. One should allow any moisture to dry because the Au can be lost due to spiting. One can do this by placing the parting cup on a hot plate to dry. Annealing the Au should be done over a flame. This turns the Au from black to gold and hardens it and causes the particles to stick together. Annealing Tips Inspect and remove foreign particles. When using a flame for the purposes of annealing, one should heat the bottom of the parting cup until it is red.

Problems The bead should not have a gold/ brass color, if it does, it means the bead is not fully parted because of the low Ag:Au ratio. For gravimetric finish one should inspect the parting cup to make sure that it is clean and weigh the sample for the same length of time as it takes to tare the balance. Flouring is when the bead breaks up during parting due because of several reasons because of incorrect Ag:Au ratio, cold parting acid, and impurities.

Fluxing and Fusion Process Description

A Description of the Fluxing and Fusion Process is simply explained once the sample is weighed and the assayer has organized as how to proceed in an orderly manner. The assayer should inspect and arrange the crucible in a fume hood. After the crucibles have been set up to the assayer liking, the assayer should determine if the sample needs to have silver added to the flux, to produce the right ratio of Ag:Au, if so silver should be added. The assayer should have by now determined the correct amount of fluxing reagents. A standard flux charge depending on the sample is as follows: One can use a 60 gram or 40 gram crucibles. The crucible should hold the charge with room to spare, as this will prevent boil over . 60 grams of litharge- 2 Tablespoons 30 grams of soda ash 1 Tablespoon 5 grams of borax 1 teaspoon If the sample is high in copper, one can use 2 grams of borax. If the sample is high in zinc and/or pyrite one tends to increase the amount of borax to 10 grams. 4 grams of silica 1 teaspoon. If the sample is high in copper, one can use 8 grams of silica. If the sample is high in zinc and/or pyrite one tends to increase the silica to 12 grams. Depending on the sample the assayer one would add either nitre, flour or perhaps nothing at all to the crucible at this stage. This is the most difficult decision, but with experience the assayer will gain the confidence to make the right choice. If in doubt, one can always ask a more experience assayer for their advice. 5 grams of nitre 1 teaspoon 4 grams of flour 1 teaspoon

One should then pour the sample in the crucible making sure the entire sample enters the crucible. One then should mix the charge as thoroughly as possible. The mixture of ore and reagents should ensure that each particle of ore is in contact with litharge and reducing agents.

Potrebbero piacerti anche