CN106501044A - Fire assaying dispensing, the method for quantitatively determining of precious metal element and pre-treating method - Google Patents
Fire assaying dispensing, the method for quantitatively determining of precious metal element and pre-treating method Download PDFInfo
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- CN106501044A CN106501044A CN201611052990.9A CN201611052990A CN106501044A CN 106501044 A CN106501044 A CN 106501044A CN 201611052990 A CN201611052990 A CN 201611052990A CN 106501044 A CN106501044 A CN 106501044A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention provides ensaying method dispensing, including following components：Sodium carbonate, lead oxide, silica, borax, silver nitrate and auxiliary material；The auxiliary material is potassium nitrate or starch；The quality of the quality of the sodium carbonate, the quality of lead oxide, the quality of silica, the quality of boric acid and silver nitrate is (25～35) with the mass ratio of prediction sample：(180～250)：(12～14)：(7～10)：(0.0005～0.01)：(5～10)；The quality of the potassium nitrate or starch is determined by the quality for predicting aimed quality that sample reducing power, fire assaying lead are buckled and the prediction sample.The Fire Assaying dispensing that the present invention is provided, cooperation between each component, it is easy to predict that the melting of sample obtains suitable size and the lead of form is buckled, ash blows, obtain noble metal and close grain, the measure that noble metal closes grain digestion solution is carried out by icp mses, realizes determining while gold, platinum and palladium element, the degree of accuracy is high.
Description
Technical field
The present invention relates to Noble Metals field, more particularly to a kind of fire assaying dispensing, the measure of precious metal element
Method and pre-treating method.
Background technology
Containing gold, platinum, palladium valuation element, the direct shadow of the height of the content of gold, platinum and palladium element in nickel ore concentrate in nickel ore concentrate
The quality judging of nickel ore concentrate is rung, therefore, the Accurate Determining of gold, platinum and palladium element is most important in nickel ore concentrate.In due to nickel ore concentrate
Matrix nickel content is high, and the relatively low degree of accuracy for causing gold, platinum and palladium constituent content mensure in nickel ore concentrate of content of gold, platinum and palladium compared with
Low, the degree of accuracy that gold, platinum and palladium three determine simultaneously is lower.
For example, often using Atomic Absorption Spectrometer (AAS) or icp mses (ICP- in prior art
MS) to ore in bullion content be measured.But, the measure for carrying out bullion content using Atomic Absorption Spectrometer
When, it is only capable of realizing the measure to certain single precious metal element content in ore, it is impossible to while multiple element is determined, and flow process
Loaded down with trivial details, less efficient, the degree of accuracy is low；And bullion content in ore is measured using Inductively coupled plasma mass spectrometry,
It is required that bullion content is higher than μ g/g levels in ore, it is difficult to complete precious metal element content in the ore relatively low to bullion content
Accurate Determining.
Content of the invention
It is an object of the invention to provide a kind of fire assaying dispensing, the assay method of precious metal element and pre-treatment side
Method, the early stage before the fire assaying dispensing for providing of the invention is easy to precious metal element to determine are processed, through the expensive of present invention offer
The pre-treating method of metallic element quantitative determination processes the sensitivity and the degree of accuracy of the measure for significantly improving precious metal element content.
The invention provides including following components：Sodium carbonate, lead oxide, silica, borax, silver nitrate and auxiliary material；Institute
Auxiliary material is stated for potassium nitrate or starch；
On the basis of predicting that the quality of sample is 5～10 parts, the sodium carbonate, lead oxide, silica, boric acid and nitric acid
Silver is (25～35) with the mass ratio of prediction sample：(180～250)：(12～14)：(7～10)：(0.0005～0.01)：(5
～10)；
The quality of the potassium nitrate or starch is by the aimed quality and prediction for predicting that the reducing power of sample, fire assaying lead are buckled
The quality of sample is obtained according to Formulas I and formula shown in formula II；
The m3Quality for the potassium nitrate；
The m4Quality for the starch；
The m5Aimed quality for fire assaying lead button；
The m6Quality for the prediction sample；
The F is the reducing power for predicting sample；
As the m3For negative value when, without potassium nitrate；As the m4For negative value when, without starch.
Preferably, on the basis of predicting that the quality of sample is 5～10 parts, the aimed quality of the fire assaying lead button is 25
～35 parts.
The invention provides a kind of pre-treating method determined for precious metal element, comprises the following steps；
A fire assaying dispensing described in above-mentioned technical proposal and prediction sample melted are obtained lead button by ()；
Ash is carried out after the b lead button demoulding that the step (a) is obtained by () to blow, noble metal is obtained and is closed grain；
C noble metal that the step (b) is obtained by () is closed grain and is mixed with nitric acid, and being mixed with chloroazotic acid after carrying out pre- clearing up is carried out
Depth is cleared up.
Preferably, the temperature of the melting of the step (a) is 1150～1170 DEG C, time of the melting is 12～
18min.
Preferably, the melt temperature is reached by way of the intensification of two steps, specially：Is sequentially passed through by initial temperature
One liter gentle second is warming up to melt temperature；
The initial temperature is 840～880 DEG C；
Described first is warming up to 980～1020 DEG C；
Described first speed for heating up is 2～6 DEG C/min；
Described second speed for heating up is 10～15 DEG C/min.
Preferably, the temperature that the ash blows is 850～880 DEG C.
Preferably, step (c) the pre- temperature that clears up be 100～150 DEG C, the pre- time that clears up be 20～
40min.
Preferably, the consumption of the nitric acid is 2～6mL.
Preferably, the consumption of the chloroazotic acid is 2～10mL.
Present invention also offers a kind of assay method of precious metal element, comprises the following steps：Using above-mentioned technical proposal
Described pre-treating method processes prediction sample, obtains predicting sample prepare liquid；Using icp mses pair
The prediction sample prepare liquid carries out the measure of precious metal element.
The invention provides ensaying method dispensing, including following components：Sodium carbonate, lead oxide, silica, borax, nitre
Sour silver and auxiliary material；The auxiliary material is potassium nitrate or starch；On the basis of predicting that the quality of sample is 5～10 parts, the sodium carbonate,
Lead oxide, silica, boric acid and silver nitrate are (25～35) with the mass ratio of prediction sample：(180～250)：(12～14)：
(7～10)：(0.0005～0.01)：(5～10)；The quality of the potassium nitrate or starch is by reducing power, the fire examination for predicting sample
The quality of the aimed quality of golden method lead button and prediction sample is obtained according to Formulas I and formula shown in formula II.The fire examination that the present invention is provided
Golden dispensing, cooperation between each raw material components, the lead for being easy to the dissolving melting for predicting sample to obtain the suitable size of aimed quality are buckled,
And the adhesion of lead button surface cladding slag is few, and the buckle-shaped state of lead is good, and lead button ash is blown, obtains noble metal and close grain, by inductive etc.
The lead button of gas ions mass spectrograph aimed quality carries out the measure that heavy metal noble metal closes grain digestion solution, during the measure of constituent content,
Realize determining while gold, three kinds of elements of platinum and palladium, and accuracy of measurement is high.The result of the embodiment of the present invention shows, adopts
Measure of the fire assaying dispensing that the present invention is provided for gold, platinum and palladium element in nickel ore concentrate, detection limit respectively 0.01g/t,
0.0004g/t, 0.004g/t, it is high that precious metal element determines sensitivity；Object element recovery of standard addition be 87.6%～
104.6%, with good accuracy of measurement；And the relative standard deviation of object element measured value is respectively less than《DZ/T
0130-2006 geological and minerals laboratory test quality management regulation》Requirement, with higher precision.
The assay method of the precious metal element that this method is provided, fire assaying is had with inductively coupled plasma mass spectrometry
Sampling amount that effect combination can take into account fire assaying is big, representative strong, stable analysis result, strong antijamming capability, concentration effect
The sensitivity of good the advantages of and inductively coupled plasma mass spectrometry is high, interference less, can Simultaneous multi element analysis advantage.
Specific embodiment
The invention provides a kind of fire assaying dispensing, including sodium carbonate, lead oxide, silica, borax, silver nitrate
And auxiliary material；The auxiliary material is potassium nitrate or starch；
On the basis of predicting that the quality of sample is 5～10 parts, the sodium carbonate, lead oxide, silica, boric acid and nitric acid
Silver is (25～35) with the mass ratio of prediction sample：(180～250)：(12～14)：(7～10)：(0.0005～0.01)：(5
～10)；
The quality of the potassium nitrate or starch is by the aimed quality and prediction for predicting that the reducing power of sample, fire assaying lead are buckled
The quality of sample is obtained according to Formulas I and formula shown in formula II；
The m3Quality for the potassium nitrate；
The m4Quality for the starch；
The m5Aimed quality for fire assaying lead button；
The m6Quality for the prediction sample；
The F is the reducing power for predicting sample；
As the m3For negative value when, without potassium nitrate；As the m4For negative value when, without starch.
The Fire Assaying dispensing that the present invention is provided, cooperation between each raw material components are easy to the dissolving for predicting sample to melt
To the suitable size of aimed quality and the lead button of form, lead button ash is blown, obtain noble metal and close grain, by inductively coupled plasma matter
The lead button of spectrometer aimed quality carries out the measure that heavy metal noble metal closes grain digestion solution, during the measure of constituent content, realizes gold, platinum
Determine with while three kinds of elements of palladium, and accuracy of measurement is high.Fire assaying by solid reagent and sample mixed, in high temperature
Lower noble metal forms the alloy containing noble metal with trapping agent, and the ratio of alloy is great, and then drops to bottom formation lead button.Sample
In base metal oxide and the flux such as gangue and silica, borax, sodium carbonate there is combination reaction, generate silicate and melt
Slag, floats over above because its density is little；Fire Assaying process simultaneously works as the double action of decomposition samples and enriching noble metals.And it is fiery
Sodium carbonate, lead oxide in preparative materials, silica, boric acid are flux, and sodium carbonate is basic solvent；Silica and boron
Sand is acidic flux, it is possible to decrease the fusing point of slag；Lead oxide is both basic solvent, is that oxidant, desulfurizing agent, noble metal are caught again
Collection agent；Silver nitrate is trapping agent.In the present invention, when in dispensing add starch when, starch as reducing agent, for by dispensing
The lead oxide of addition is reduced into lead, traps noble metal whereby；When potassium nitrate is added in dispensing, potassium nitrate is used as oxidant
Enter in slag in the sulfide-oxidation in sample into oxide, to be made metal oxide.
The fire assaying dispensing that the present invention is provided, including sodium carbonate, lead oxide, silica, borax, silver nitrate and and
Auxiliary material；The auxiliary material is potassium nitrate or starch.The present invention does not have special restriction to the source of detection sample and species, the present invention
The dispensing of offer can be used in sulphide ore material well known to those skilled in the art, in the present invention, the fire assaying pre-
Test sample product for nickel ore concentrate material, silicate, carbonate, sulphide ore, oxide ore, chromite, olivine pyroxenolite or can select smelting concentrate
Material.In the present invention, the group of the nickel ore concentrate be divided into the mass ratio of nickel, copper, iron, magnesia, silica and sulphur for (8～
10)：(0.5～2)：(20～30)：(10～20)：(25～40)：The nickel ore concentrate or nickel of (15～20), copper, iron, magnesia, two
The mass ratio of silica and sulphur is (8～10)：(3～6)：(30～50)：(0.5～3)：(10～20)：The nickel essence of (20～40)
Ore deposit.The present invention does not have particular/special requirement to the source of the nickel ore concentrate material, using nickel ore concentrate well-known to those skilled in the art
?.
In the present invention, on the basis of predicting that the quality of sample is 5～10 parts, the sodium carbonate, lead oxide, titanium dioxide
Silicon, boric acid and silver nitrate are (25～35) with the mass ratio of prediction sample：(180～250)：(12～14)：(7～10)：
(0.0005～0.01)：(5～10), preferably (28～32)：(190～225)：(12.5～13.5)：(8～8.5)：(0.001
～0.002)：(6～7).
In the present invention, the fire assaying dispensing, in parts by weight, prediction sample described in techniques described above scheme
25～35 parts of sodium carbonate is preferably included on the basis of 5～10 weight portions, and more preferably 28～32 parts, be even more preferably 30
Part.The present invention does not have particular/special requirement to the source of the sodium carbonate, using well-known to those skilled in the art.
The fire assaying dispensing that the present invention is provided, in parts by weight, predicts the 5～10 of sample described in techniques described above scheme
On the basis of weight portion, including 180～250 parts of lead oxide, preferably 190～225 parts, more preferably 200 parts.At this
In bright, the lead oxide is preferably powdery lead oxide；In the present invention, the particle diameter of the lead oxide is preferably 0.5～3 μm.?
In the present invention, the lead oxide is preferably the lead oxide of gold ＜ 0.25g/kg, platinum ＜ 0.25g/kg and palladium ＜ 0.25g/kg.This
The bright source to the lead oxide does not have particular/special requirement, using yellow lead oxide well-known to those skilled in the art.
The fire assaying dispensing that the present invention is provided, in parts by weight, predicts the 5～10 of sample described in techniques described above scheme
On the basis of weight portion, including 12～14 parts of silica, preferably 12.5～13.5 parts, more preferably 13 parts.This
The bright source to the silica does not have particular/special requirement, using silica well-known to those skilled in the art.
The fire assaying dispensing that the present invention is provided, in parts by weight, predicts the 5～10 of sample described in techniques described above scheme
On the basis of weight portion, 7～9 parts of borax preferably included, more preferably 8～8.5 parts.Source of the present invention to the borax
Without particular/special requirement, using borax well-known to those skilled in the art.In an embodiment of the present invention, the borax tool
Body selects borax commercially available prod.
The fire assaying dispensing that the present invention is provided, in parts by weight, predicts the 5～10 of sample described in techniques described above scheme
On the basis of weight portion, including 0.0005～0.01 part of silver nitrate, preferably 0.001～0.005 part.In the present invention, the nitre
Sour silver is added preferably in the form of silver nitrate solution.The present invention does not have special wanting to the concentration and volume of the silver nitrate solution
Ask, be defined so that the silver nitrate for limiting mass parts can be provided.In an embodiment of the present invention, the concentration of the silver nitrate solution is preferred
For 1～10g/L, more preferably 6～8g/L.
The fire assaying dispensing that the present invention is provided, including auxiliary material, the auxiliary material is potassium nitrate or starch.In the present invention,
The quality of the potassium nitrate or starch is by the matter for predicting aimed quality that the reducing power of sample, fire assaying lead are buckled and prediction sample
Amount is obtained according to Formulas I and formula shown in formula II；
The m3Quality for the potassium nitrate；
The m4Quality for the starch；
The m5Aimed quality for fire assaying lead button；
The m6Quality for the prediction sample；
The F is the reducing power for predicting sample；
As the m3For negative value when, without potassium nitrate；As the m4For negative value when, without starch.
In the present invention, the prediction sample reducing power is preferably determined using reducing power test, described in the present invention pre-
Test sample product reducing power is preferably the quality of the sample that the reducing power test is added and the reducing power is tested the lead for obtaining and buckles matter
The ratio of amount.The present invention does not have particular/special requirement to the prediction sample reducing power test, using well-known to those skilled in the art
The reducing power test of prediction sample.In an embodiment of the present invention, the prediction sample reducing power test is specially：5g is pre-
980 are warming up to from 850 DEG C in 40min after the mixing of test specimens, 10g sodium carbonate, 60g lead oxide, 5g silica and 5g boraxs
DEG C～1020 DEG C, being melted after being directly warming up to 1160 DEG C again in 5～10min, the time of the melting is preferably
15min；The fused mass for obtaining is cooled to isolated lead button after 20～25 DEG C after completing the melting.In the present invention, institute
State prediction sample identical with the prediction sample source of the fire assaying；In the present invention, the sodium carbonate, lead oxide, dioxy
SiClx and borax are preferably defined according to above-mentioned technical proposal.The present invention does not have particular/special requirement to the detached mode, adopts
With separate mode well-known to those skilled in the art.Isolated lead button described in preferred pair of the present invention carries out surface and melts
The quality of the lead button is weighed after the removing of slag；The present invention does not have particular/special requirement to the reset mode of the surface slag, adopts
Slag reset mode in surface well-known to those skilled in the art.
The quality that the lead button quality that reducing power test is obtained tests the sample for adding with the reducing power substitutes into formula
Formula shown in III, obtains predicting sample reducing power：
M described in formula III1For the quality that the reducing power tests the sample for adding；The m2Test for the reducing power
The lead button quality for arriving；The F is the prediction sample reducing power.
On the basis of the present invention is 5～10 parts by the quality for predicting sample, the aimed quality of the fire assaying lead button is preferred
For 25～35 parts, more preferably 28～32 parts, more preferably 30 parts.
After obtaining the aimed quality that the prediction sample reducing power and fire assaying lead are buckled, the present invention is gone back by prediction sample
Former power, the aimed quality of fire assaying lead button and prediction sample quality according to Formulas I and formula shown in formula II obtain potassium nitrate or
The quality of starch.The present invention determines interpolation potassium nitrate or starch with the quality of the potassium nitrate for obtaining and starch；When the nitre
When the quality of sour potassium is negative value, the present invention adds starch preferably without potassium nitrate, and the quality of the starch is preferably above-mentioned public affairs
The quality of the starch that formula determines；When the quality of the starch is negative value, the present invention adds potassium nitrate preferably without starch,
The quality of the potassium nitrate is preferably the quality of the potassium nitrate that above-mentioned formula determines.
The invention provides the pre-treating method determined for precious metal element, comprises the following steps：
A Fire Assaying dispensing described in above-mentioned technical proposal and prediction sample melted are obtained lead button by ()；
Ash is carried out after the b lead button demoulding that the step (a) is obtained by () to blow, noble metal is obtained and is closed grain；
C noble metal that the step (b) is obtained by () is closed grain and is mixed with nitric acid, and being mixed with chloroazotic acid after carrying out pre- clearing up is carried out
Depth is cleared up.
Fire Assaying dispensing described in above-mentioned technical proposal and prediction sample melted are obtained lead button by the present invention.The present invention is excellent
After choosing is by the prediction sample, sodium carbonate, lead oxide, silica, borax and potassium nitrate or starch mixing, the nitre is added
Sour silver solution.In the present invention, the container of the mixing is preferably scorifier.The present invention does not have spy to the mode of the mixing
Different requirement, using the hybrid mode of fire assaying dispensing well-known to those skilled in the art；After completing the mixing, this
The silver nitrate solution is preferably added to the zone line of the mixture, in an embodiment of the present invention, the nitre for invention
The interpolation form of sour silver solution is specially：In the pit-hole that the zone line of the mixed material for obtaining forms a diameter of 2～5mm
Afterwards the silver nitrate solution is added.
In the present invention, the temperature of the melting is preferably 1150～1170 DEG C, more preferably 1160～1165 DEG C；
In the present invention, the time of the melting is preferably 12～18min, most preferably more preferably 13～16min, 15min.
In the present invention, the melt temperature is preferably reached by way of the intensification of two steps, specially：By initial temperature according to
Secondary melt temperature is warming up to through first liter gentle second.
In the present invention, the initial temperature is preferably 840～880 DEG C, more preferably 850～860 DEG C；At this
In bright, described first heats up preferably is warming up to 980～1020 DEG C, more preferably 1000～1010 DEG C；In the present invention, institute
The speed for stating first step intensification is preferably 2～6 DEG C/min, more preferably 4～5 DEG C/min；In the present invention, described first
The time that step heats up is preferably 30～50min, more preferably 40min.In the present invention, second step heats up and is preferably warming up to
1100～1200 DEG C, more preferably 1160 DEG C, the speed that the second step heats up is preferably 10～15 DEG C/min, further
Preferably 13～14 DEG C/min.
After obtaining fused mass, the present invention is separated after preferably cooled down the fused mass, obtains lead button.Of the invention preferred
Cooled down using the fused mass is placed in pig mold；In the present invention, the temperature after the cooling is preferably 20～25
℃.The present invention does not have particular/special requirement to the detached mode, using the type of cooling well-known to those skilled in the art.
After obtaining the lead button, weigh after the surface scum for preferably removing the lead button of the invention.The present invention is to the table
The reset mode of face scum silica frost does not have particular/special requirement, using surface scum reset mode well-known to those skilled in the art.
In the present invention, the quality of the lead button is preferably 25～35g, more preferably 30～32g.
The present invention passes through to control potassium nitrate or flour in the consumption of dispensing component and dispensing, in conjunction with potassium nitrate or flour
Concrete consumption in dispensing, obtains the lead button that any surface finish degree is high, lead button surface slag clearance is high, and then improves expensive
The rate of recovery of metal.
The present invention will carry out ash after the lead button demoulding for obtaining and blow, and obtains noble metal and closes grain.The present invention is preferably 880～920
DEG C insulation 3～6min complete the demoulding, further preferably 900 DEG C insulation 4～5min complete the demoulding；In the present invention, described de-
The temperature of mould preferably passes through to reach in 880～920 DEG C of preheating more than 20min；Time of the preheating more preferably 30～
40min.In an embodiment of the present invention, the process of the demoulding is specifically carried out in the magnesia cupel being placed in cupel(lation) furnace；?
In the knockout course, the cupel(lation) furnace preferably is off fire door.
After completing the demoulding, carry out ash and blow.In the present invention, the temperature that the ash blows is preferably 850～880 DEG C, enters
One step is preferably 860～865 DEG C.In the present invention, the temperature that the ash blows increases with the minimizing of lead button quality.In the present invention
In, the ash blows and preferably completes in cupel(lation) furnace；In the present invention, the temperature that the ash blows is preferably using the opening fire door
Mode reaches.The present invention does not have particular/special requirement to the time that the ash blows, with seeing that noble metal is closed after glistening occurs in grain.
The noble metal for obtaining conjunction grain is mixed by the present invention with nitric acid, carry out pre- clear up carry out depth and disappear
Solution.In the present invention, the consumption of the nitric acid is preferably 2～6mL, more preferably 4～6mL.In the present invention, the nitre
L.42g/mL the density of acid be preferably, and the present invention does not have particular/special requirement to the source of the nitric acid, using those skilled in the art
Known nitric acid；In an embodiment of the present invention, the nitric acid is specially commercially available nitric acid (ρ=l.42g/mL), top grade
Pure.
Noble metal described in preferred pair of the present invention closes grain and carries out cleaning post-drying, then mixes with nitric acid.In the present invention, described
The preferably acetic acid boiling of the mode of cleaning is boiled and is cleaned with distilled water successively；In the present invention, the time that the acetic acid boiling is boiled is preferably
10～15min, more preferably 12～13min；In the present invention, it is l.05g/mL commercially available that the acetic acid is preferably density
The mixed liquor of acetic acid and water, it is 1 with the ratio of water that density is commercially available acetic acid l.05g/mL:3；In the present invention, the acetic acid
Consumption preferably by can realize to the noble metal close grain immersion be defined.
After completing the noble metal conjunction grain and nitric acid mixing, the compound for obtaining is carried out pre- clearing up by the present invention.At this
In bright, the pre- temperature that clears up is preferably 100～150 DEG C, more preferably 120～130 DEG C；In the present invention, described
The time that clears up in advance is preferably 20～40min, more preferably 25～30min.In the present invention, described pre- clear up preferably
Micro-wave digestion；In the present invention, the power of the micro-wave digestion preferably 800～1500W, more preferably 1000～
1200W；In the present invention, the rate of climb time of the micro-wave digestion is preferably 10～15min；In the present invention, described micro-
The retention time that ripple is cleared up is preferably 10～30min.In the present invention, pre- the clearing up is carried out preferably in micro-wave diminishing pot.
The present invention by described pre- clear up product and mix with chloroazotic acid carry out depth and clear up.In the present invention, the body of the chloroazotic acid
Product is preferably 4～10mL, more preferably 6～10mL.In the present invention, described pre- clear up after product is mixed with chloroazotic acid preferably
Stood, the time of the standing is preferably 30～40min；In the present invention, described pre- disappear is completed during the standing
Solution product and the reaction of chloroazotic acid, produce bubble, realize clearing up.After completing the standing, present invention preferably employs heating using microwave
Mode carries out depth and clears up；In the present invention, the time that the depth is cleared up is preferably 30～40min, and the depth is cleared up
Temperature is preferably 130～140 DEG C.The present invention does not have particular/special requirement to the mode of the heating using microwave, using people in the art
The mode of the heating using microwave known to member.
Present invention also offers the assay method of noble metal, comprises the following steps：Before described in above-mentioned technical proposal
Disposal methods predict sample, obtain predicting sample prepare liquid；Using icp mses to the prediction
Sample prepare liquid carries out the measure of precious metal element.
The present invention processes prediction sample using the pre-treating method described in above-mentioned technical proposal, obtains predicting that sample is to be measured
Liquid.
After obtaining the prediction sample prepare liquid, the present invention carries out precious metal element using Inductively coupled plasma mass spectrometry
Measure.Inductively coupled plasma mass spectrometry described in preferred pair of the present invention is tuned；The present invention is not special to the tuning
Require, using mass spectrograph tuning manner well-known to those skilled in the art, so that the Inductively coupled plasma mass spectrometry
Sensitivity, oxide, double charge, background value and resolution ratio index reach precious metal element well-known to those skilled in the art
Determine and require.
After completing the tuning, preferred pair standard liquid of the present invention, blank solution and prediction sample solution to be measured carry out unit
The measure of element, obtains the content of the prediction Gold Samples, platinum and palladium element.In the present invention, the standard liquid is preferably pressed
Prepared according to STD1～STD6 in table 1.
In the present invention, the measure of the blank solution is used for eliminating the target element introduced when adding reagent in process of the test
The interference of element.The present invention does not have particular/special requirement to the preparation of the blank solution, using sky well-known to those skilled in the art
The preparation method of white solution；In an embodiment of the present invention, the preparation method of the blank solution is specially：According to above-mentioned
The preparation method for predicting sample solution to be measured described in technical scheme is obtained, with prediction sample solution preparation method to be measured
By described fire assaying dispensing and prediction sample melted when difference is prepared by prediction sample solution to be measured, lead is obtained
Button；The fire assaying is melted with dispensing when prepared by the blank solution, obtain lead button.
The present invention preferably adds internal standard element, institute in the standard liquid, blank solution and prediction sample solution to be measured
State internal standard element and be preferably yttrium and/or thorium.In the present invention, the addition of the internal standard element is adding the mark after internal standard element
The densimeter of internal standard element in quasi- solution, blank solution and prediction sample solution to be measured；In the present invention, the addition internal standard unit
In standard liquid, blank solution and prediction sample solution to be measured after element, the concentration of yttrium is independently preferably 10～100ng/mL,
More preferably 20～60ng/mL, more preferably 25ng/mL；Standard in the present invention, after the addition internal standard element
In solution, blank solution and prediction sample solution to be measured, the concentration of thorium is independently preferably 10～100ng/mL, further preferably
For 20～60ng/mL, more preferably 25ng/mL.In the present invention, in prediction sample solution to be measured, internal standard element can be in your gold
Add in the pretreatment process of category element quantitative determination, it is also possible to add during Instrument measuring.
Described in preferred pair of the present invention, standard liquid carries out element determination, obtains constituent content matched curve；Obtain element to contain
After amount matched curve, preferred pair of the present invention predicts that sample solution to be measured carries out element determination, with the constituent content matched curve
Carry out compareing the content for obtaining prediction sample GOLD FROM PLATING SOLUTION to be measured, platinum and palladium element.
1 standard liquid of table and blank solution
The present invention carries out mass spectrum interference preferably by isotopic element calibration equation to the Inductively coupled plasma mass spectrometry
Eliminate.The present invention does not have particular/special requirement to the cancellation that the mass spectrum is disturbed, using side well-known to those skilled in the art
Formula.
The present invention does not have particular/special requirement to the type of the icp mses, using people in the art
Inductively coupled plasma mass spectrometry known to member.Condition of work of the present invention to the Inductively coupled plasma mass spectrometry
Without particular/special requirement, using the condition of work of Inductively coupled plasma mass spectrometry well-known to those skilled in the art, according to not
Require to limit with the condition of equipment.In an embodiment of the present invention, the condition of work tool of the Inductively coupled plasma mass spectrometry
Body is limited according to the requirement in table 2.
2 icp mses condition of work of table
In the present invention, the mass number determined by the element to be measured and internal standard element is shown in Table 3.In the present invention, described
Under mass number, mass spectrograph determines sensitivity height, and interference is little, and mass number is a crucial inductivity coupled plasma mass spectrometry of comparison
The location parameter of instrument.
3 element to be measured of table and internal standard element quality measurement number
| Element | Au | Pt | Pd |
| Mass number | 197 | 195 | 106 |
| From internal standard element | 232Th | 232Th | 89Y |
The invention provides ensaying method dispensing, including following components：Sodium carbonate, lead oxide, silica, borax, nitre
Sour silver and auxiliary material；The auxiliary material is potassium nitrate or starch；On the basis of predicting that the quality of sample is 5～10 parts, the sodium carbonate,
Lead oxide, silica, boric acid and silver nitrate are (25～35) with the mass ratio of prediction sample：(180～250)：(12～14)：
(7～10)：(0.0005～0.01)：(5～10)；The quality of the potassium nitrate or starch is by reducing power, the fire examination for predicting sample
The quality of the aimed quality of golden method lead button and prediction sample is obtained according to Formulas I and formula shown in formula II.The fire examination that the present invention is provided
Golden dispensing, cooperation between each raw material components are easy to predict that the dissolving of sample obtains the lead of aimed quality and buckles, by aimed quality
Lead button carry out precious metal element content measure when, realize determining while gold, three kinds of elements of platinum and palladium, and determine accurately
Degree is high.The result of the embodiment of the present invention shows that the fire assaying dispensing provided using the present invention is for gold, platinum and palladium in nickel ore concentrate
The measure of element, detection limit are respectively 0.01g/t, 0.0004g/t, 0.004g/t, and it is high that precious metal element determines sensitivity；Target
Element recovery of standard addition is 87.6%～104.6%, with good accuracy of measurement；And object element measured value is relative
Standard deviation is respectively less than《DZ/T 0130-2006 geological and minerals laboratory test quality management regulation》Requirement, with higher
Precision.In order to further illustrate the present invention, with reference to fire assaying dispensing, noble metal of the embodiment to present invention offer
The method for quantitatively determining and pre-treating method of element is described in detail, but they can not be interpreted as to present invention protection model
The restriction that encloses.
Embodiment 1
Fire assaying dispensing：
Reducing power is tested：5g samples, 10g sodium carbonate, 60g lead oxide, 5g silica, 5g boraxs are weighed in scorifier
Middle mixing.Crucible with honest material is placed in 850 DEG C of ensaying electric furnace, 1000 DEG C is to slowly warm up in 40min, subsequent 10min
1160 DEG C are inside warming up to, keeping temperature is stable, melting 15min comes out of the stove.Fused mass is poured in pig mold, 25 DEG C are cooled to, from
Lead button is isolated in slag.Lead button surface attachment slag is removed, and lead button quality is weighed for 28 grams.According to sample mass and lead button matter
Amount is made the mode of ratio and obtains reducing power F for 5.6.
Determine fire assaying lead button aimed quality be 25g, prediction sample quality be defined as 5g, by the reducing power F for obtaining,
The quality of the aimed quality of fire assaying lead button and prediction sample substitutes into Formulas I and formula II：
Obtain m3For 0.75g, m4For -0.25g.And then determine addition potassium nitrate 0.75g in fire assaying dispensing.
Weigh 5g prediction samples, add 30g sodium carbonate, 200g lead oxide, 13g silica, 8.5g boraxs, 0.75g nitre
Sour potassium after being well mixed, digs a pitting in mixed material zone line with little spoon in scorifier, and 100 μ L concentration of addition are
The silver nitrate solution of 10g/L, obtains Fire Assaying dispensing.
The Fire Assaying dispensing for obtaining is placed in crucible, crucible is placed in 840 DEG C of ensaying electric furnace, with 4 in 40min
DEG C/ramp of min to 1000 DEG C, with the ramp of 10 DEG C/min to 1150 DEG C, insulation 12min goes out after being melted
Stove.Fused mass is poured in pig mold.25 DEG C are cooled to, and lead button is isolated from slag.Lead button surface attachment slag is removed, and
Weigh and obtain lead button 26g.
The lead button for obtaining is put in the magnesia cupel for 20min being preheated in 880 DEG C of cupel(lation) furnaces, fire door is closed, and melts 3
～6min demouldings, realize complete demoulding, open fire door, are cooled to 850 DEG C and carry out ash and blow, flash of light occur when grain is closed in magnesia cupel
Cupel can be taken out afterwards, be put in cupel tray.
Noble metal is taken out from cupel closes grain, flat with hand hammer hammer on clean anvil, it is put in the porcelain crucible of 25mL, plus
Enter 20mL acetic acid and boil 10min, be poured off acetic acid, grain is closed with distillation water washing noble metal and dried.Noble metal is closed grain to move into
In micro-wave diminishing pot, add 4mL nitric acid, clear up 30min in advance for 120 DEG C on the control-temperature electric heating plate, then in micro-wave diminishing pot plus
Enter 6mL chloroazotic acid, place half an hour and treat that vigorous reaction stops, adding a cover set, be placed in rotating disk, be put in furnace chamber, start micro-wave digestion,
The depth for carrying out 70min is cleared up.To be cooled, it is transferred in 50mL volumetric flasks with water, is diluted with water to scale, is mixed, stand
To prediction sample liquid, and internal standard element yttrium and thorium is added so that in prediction sample liquid, the concentration of yttrium is 25ng/mL, the concentration of thorium
For 25ng/mL.
Blank solution is prepared according to above-mentioned preparation prediction sample liquid mode, is differed only in and need not be added 5g samples, obtain
After blank solution, internal standard element yttrium and thorium is added so that in blank solution, the concentration of yttrium is 25ng/mL, and the concentration of thorium is 25ng/
mL.
Set isotopic element calibration equation and mass spectrographic interference is eliminated to Inductively coupled plasma mass spectrometry.To inductive etc. from
Sub- mass spectrograph is tuned, and is defined according to condition of work shown in table 2.According to 1 preparing standard solution of table, and add internal standard unit
Plain yttrium and thorium, in standard liquid, the concentration of yttrium is 25ng/mL, and the concentration of thorium is 25ng/mL, enters row element survey to standard liquid
Fixed, obtain constituent content matched curve (Au：Y=0.0134x+0.0467；Pt：Y=0.0086x-0.0071, Pd：Y=
0.0090x+0.0054).
To predicting that sample liquid and blank solution carry out element determination, prediction sample liquid and the constituent content matched curve
Compareed, and reagent interference is excluded by the measure of blank solution, obtained prediction sample GOLD FROM PLATING SOLUTION to be measured, platinum and palladium
The content of element is respectively 69.52ng/mL, 53.10ng/mL and 204.21ng/mL, then prediction Gold Samples, platinum and palladium element
Content be respectively 0.70g/t, 0.53g/t and 2.04g/t.
Recovery testu is carried out using Au, Pt and Pd for adding 2.50 μ g and 5.00 μ g in sample, obtain Au, Pt and
The recovery of standard addition of Pd is respectively 91.6%, 97.9% and 87.6%, with good accuracy of measurement.
Precision is calculated by 11 independent experiments to sample, the relative standard deviation of Au, Pt and Pd measured value is obtained
For 9.8%, 9.5% and 3.3%.
The measure of gold, platinum and palladium element in nickel ore concentrate, detection limit are respectively 0.01g/t, 0.004g/t, 0.004g/t, spirit
Quick height.
Embodiment 2
Fire assaying dispensing：
Reducing power is tested：5g samples, 10g sodium carbonate, 60g lead oxide, 5g silica, 5g boraxs are weighed in scorifier
Middle mixing.Crucible with honest material is placed in 850 DEG C of ensaying electric furnace, 1000 DEG C is to slowly warm up in 40min, subsequent 10min
1160 DEG C are inside warming up to, keeping temperature is stable, melting 15min comes out of the stove.Fused mass is poured in pig mold, 25 DEG C are cooled to, from
Lead button is isolated in slag.Lead button surface attachment slag is removed, and lead button quality is weighed for 11 grams.According to sample mass and lead button matter
Amount is made the mode of ratio and obtains reducing power F for 2.2.
Determine fire assaying lead button aimed quality be 30g, prediction sample quality be defined as 10g, by the reducing power for obtaining
The quality of F, the aimed quality of fire assaying lead button and prediction sample substitutes into Formulas I and formula II：
Obtain m3For -2.00g, m4For 0.67g.And then determine addition starch 0.67g in fire assaying dispensing.
Weigh 10g prediction samples, add 30g sodium carbonate, 200g lead oxide, 13g silica, 8.5g boraxs, 0.67g to form sediment
Powder after being well mixed, digs a pitting in mixed material zone line with little spoon in scorifier, and 100 μ L concentration of addition are
The silver nitrate solution of 10g/L, obtains Fire Assaying dispensing.
The Fire Assaying dispensing for obtaining is placed in crucible, crucible is placed in 840 DEG C of ensaying electric furnace, with 4 in 40min
DEG C/ramp of min to 1000 DEG C, with the ramp of 10 DEG C/min to 1150 DEG C, insulation 15min goes out after being melted
Stove.Fused mass is poured in pig mold.25 DEG C are cooled to, and lead button is isolated from slag.Lead button surface attachment slag is removed, and
Weigh and obtain lead button 31g.
The lead button for obtaining is put in the magnesia cupel for 20min being preheated in 880 DEG C of cupel(lation) furnaces, fire door is closed, and is melted
5min demouldings, realize complete demoulding, open fire door, are cooled to 850 DEG C and carry out ash and blow, after closing grain in magnesia cupel and flash of light occur
Cupel can be taken out, be put in cupel tray.
Noble metal is taken out from cupel closes grain, flat with hand hammer hammer on clean anvil, it is put in the porcelain crucible of 25mL, plus
Enter 20mL acetic acid and boil 10min, be poured off acetic acid, grain is closed with distillation water washing noble metal and dried.Noble metal is closed grain to move into
In micro-wave diminishing pot, add 4mL nitric acid, clear up 30min in advance for 120 DEG C on the control-temperature electric heating plate, then in micro-wave diminishing pot plus
Enter 6mL chloroazotic acid, place half an hour and treat that vigorous reaction stops, adding a cover set, be placed in rotating disk, be put in furnace chamber, start micro-wave digestion,
The depth for carrying out 70min is cleared up.To be cooled, it is transferred in 50mL volumetric flasks with water, is diluted with water to scale, is mixed, stand
To prediction sample liquid, and internal standard element yttrium and thorium is added so that in prediction sample liquid, the concentration of yttrium is 100ng/mL, the concentration of thorium
For 100ng/mL.
Blank solution is prepared according to above-mentioned preparation prediction sample liquid mode, is differed only in and need not be added 5g samples, obtain
After blank solution, internal standard element yttrium and thorium is added so that the concentration of yttrium is 100ng/mL in blank solution, the concentration of thorium is
100ng/mL.
Set isotopic element calibration equation and mass spectrographic interference is eliminated to Inductively coupled plasma mass spectrometry.To inductive etc. from
Sub- mass spectrograph is tuned, and is defined according to condition of work shown in table 2.After according to 1 preparing standard solution of table, and add internal standard
Yt and thorium, in standard liquid, the concentration of yttrium is 100ng/mL, and the concentration of thorium is 100ng/mL.Row element is entered to standard liquid
Determine, obtain constituent content matched curve (Au：Y=0.0135x+0.0039；Pt：Y=0.0086x+0.0004, Pd：Y=
0.0091x+0.0033).To predicting that sample liquid and blank solution carry out element determination, prediction sample liquid and the constituent content
Matched curve is compareed, and excludes reagent interference by the measure of blank solution, is obtained in prediction sample solution to be measured
The content of gold, platinum and palladium element is respectively 62.28ng/mL, 47.34ng/mL and 38.67ng/mL, then prediction Gold Samples, platinum
0.31g/t, 0.24g/t and 0.19g/t are respectively with the content of palladium element.
Recovery testu is carried out using Au, Pt and Pd for adding 1.50 μ g and 3.00 μ g in sample, obtain Au, Pt and
The recovery of standard addition of Pd is respectively 103.2%, 91.4% and 92.5%, with good accuracy of measurement.
The measure of gold, platinum and palladium element in nickel ore concentrate, detection limit are respectively 0.01g/t, 0.001g/t, 0.001g/t, spirit
Sensitivity is high.
Precision is calculated by 11 independent experiments to sample, the relative standard deviation of Au, Pt and Pd measured value is obtained
For 11.3%, 6.7% and 4.2%, it is less than《DZ/T 0130-2006 geological and minerals laboratory test quality management regulation》Will
Ask, with higher precision.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of fire assaying dispensing, including following components：Sodium carbonate, lead oxide, silica, borax, silver nitrate and auxiliary
Material；The auxiliary material is potassium nitrate or starch；
By predict sample quality be 5～10 parts on the basis of, the sodium carbonate, lead oxide, silica, boric acid and silver nitrate with
The mass ratio of prediction sample is (25～35)：(180～250)：(12～14)：(7～10)：(0.0005～0.01)：(5～
10)；
The quality of the potassium nitrate or starch is by the aimed quality and prediction sample for predicting that the reducing power of sample, fire assaying lead are buckled
Quality obtain according to Formulas I and formula shown in formula II；
The m3Quality for the potassium nitrate；
The m4Quality for the starch；
The m5Aimed quality for fire assaying lead button；
The m6Quality for the prediction sample；
The F is the reducing power for predicting sample；
As the m3For negative value when, without potassium nitrate；As the m4For negative value when, without starch.
2. fire assaying dispensing according to claim 1, it is characterised in that to predict the quality of sample as 5～10 parts
On the basis of, the aimed quality of the fire assaying lead button is 25～35 parts.
3. a kind of pre-treating method for precious metal element quantitative determination, comprises the following steps；
A fire assaying dispensing described in claim 1 and 2 any one and prediction sample melted are obtained lead button by ()；
Ash is carried out after the b lead button demoulding that the step (a) is obtained by () to blow, noble metal is obtained and is closed grain；
C noble metal that the step (b) is obtained by () is closed grain and is mixed with nitric acid, and mixing with chloroazotic acid after carrying out pre- clearing up carries out depth
Clear up.
4. pre-treating method according to claim 3, it is characterised in that the temperature of the melting of the step (a) is 1150
～1170 DEG C, the time of the melting is 12～18min.
5. the pre-treating method according to claim 3 or 4, it is characterised in that the melt temperature is heated up by two steps
Mode reaches, specially：First liter gentle second is sequentially passed through by initial temperature and is warming up to melt temperature；
The initial temperature is 840～880 DEG C；
Described first is warming up to 980～1020 DEG C；
Described first speed for heating up is 2～6 DEG C/min；
Described second speed for heating up is 10～15 DEG C/min.
6. pre-treating method according to claim 3, it is characterised in that the temperature that the ash blows is 850～880 DEG C.
7. pre-treating method according to claim 3, it is characterised in that step (c) the pre- temperature that clears up is 100～
150 DEG C, the pre- time that clears up is 20～40min.
8. the pre-treating method according to claim 3 or 7, it is characterised in that the consumption of the nitric acid is 2～6mL.
9. pre-treating method according to claim 8, it is characterised in that the consumption of the chloroazotic acid is 2～10mL.
10. a kind of method for quantitatively determining of precious metal element, comprises the following steps：
Prediction sample is processed using the pre-treating method described in any one of claim 4～9, obtains predicting sample prepare liquid；
The measure that heavy metal element is carried out to the prediction sample prepare liquid using icp mses.
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| CN107991207A (en) * | 2017-11-29 | 2018-05-04 | 长春黄金研究院 | Golden assay method in a kind of high impurity copper anode mud |
| CN109916763A (en) * | 2019-03-15 | 2019-06-21 | 嵩县金牛有限责任公司 | A method of gold dollar cellulose content is analyzed using Fire Assaying |
| CN109975164A (en) * | 2019-03-25 | 2019-07-05 | 昆山全亚冠环保科技有限公司 | The Fire Assaying analysis method of gold-containing solution |
| CN113092305A (en) * | 2021-04-12 | 2021-07-09 | 北矿检测技术有限公司 | Method for detecting gold content in coarse impure copper and application |
| CN114152489A (en) * | 2021-11-16 | 2022-03-08 | 河南省岩石矿物测试中心 | Platinum-palladium-gold gray blowing method in black rock by taking tellurium and silver as protective agent |
| CN114152489B (en) * | 2021-11-16 | 2024-05-03 | 河南省岩石矿物测试中心 | Platinum-palladium-gold gray blowing method in black rock by taking tellurium-silver as protective agent |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107991207A (en) * | 2017-11-29 | 2018-05-04 | 长春黄金研究院 | Golden assay method in a kind of high impurity copper anode mud |
| CN109916763A (en) * | 2019-03-15 | 2019-06-21 | 嵩县金牛有限责任公司 | A method of gold dollar cellulose content is analyzed using Fire Assaying |
| CN109975164A (en) * | 2019-03-25 | 2019-07-05 | 昆山全亚冠环保科技有限公司 | The Fire Assaying analysis method of gold-containing solution |
| CN113092305A (en) * | 2021-04-12 | 2021-07-09 | 北矿检测技术有限公司 | Method for detecting gold content in coarse impure copper and application |
| CN114152489A (en) * | 2021-11-16 | 2022-03-08 | 河南省岩石矿物测试中心 | Platinum-palladium-gold gray blowing method in black rock by taking tellurium and silver as protective agent |
| CN114152489B (en) * | 2021-11-16 | 2024-05-03 | 河南省岩石矿物测试中心 | Platinum-palladium-gold gray blowing method in black rock by taking tellurium-silver as protective agent |
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Application publication date: 20170315 |