CN107478765A - A kind of nickel-silicon nitride method in thick gold - Google Patents
A kind of nickel-silicon nitride method in thick gold Download PDFInfo
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Abstract
The present invention relates to a kind of nickel-silicon nitride method in thick gold, belong to the assay method of nickel amount in thick gold.With aqua regia dissolution sample, separation gold is precipitated with hydrazine hydrate, filtering, filter residue are used for reclaiming gold, ammonium chloride are added in filtrate and ammoniacal liquor forms alkaline buffer system, add dimethylglyoxime precipitation separation nickel, using hexamethylenetetramine as cushioning liquid, excessive EDTA and nickel reactant are added, excessive EDTA is using xylenol orange as indicator, it is terminal that zinc chloride, which is that titrant is titrated to solution to be changed into purplish red from yellow, calculates the content of nickel in thick gold.The present invention can be adapted to high-volume to analyze, while filled up the blank of nickel quantity measuring method in thick gold with the content of nickel in the thick gold of Accurate Determining.
Description
Technical field
The invention belongs to a kind of nickel-silicon nitride method in thick gold, especially suitable for the thick gold containing various metals impurity simultaneously
The batch measure of middle nickel content.
Background technology
In thick golden product standard YS/T3026-2016, two ranks of mass fraction point of the thick golden down payment after melting, its
Chemical composition should meet the regulation of table 1.
The chemical composition of the thick gold after melting of table 1
The regulation not detected only has been done to mercury and iridium in standard, only total impurities provided in addition, and to impurity
The impurity element that species defines detection includes but is not limited to impurity element listed by table 1.
Obtained by enterprise's investigation and analysis, common at present thick gold and impurity element are：Silver, copper, zinc and nickel.Wherein nickel contains
Measure as Ni:0.522%~17.1%.But there was only the measure of gold amount and silver amount in thick gold, neither one at present in examination criteria
For the method for nickel-silicon nitride in thick gold.Therefore, invention one kind is suitable for batch detection and accurately and reliably method is thick to determine
Nickel amount has very great meaning in gold.
The content of the invention
The present invention provides a kind of nickel-silicon nitride method in thick gold, does not have suitable detection method to solve high content nickel in thick gold
The problem of, it is therefore an objective to find it is a kind of can in the thick gold of Accurate Determining the amount suitable batch operation again of nickel method.
The present invention adopts the technical scheme that, comprises the following steps：
(1) appropriate sample is weighed, is placed in 250mL beakers, adds 10mL chloroazotic acid, cap upper surface ware, low-temperature heat to examination
Sample is completely dissolved, addition 1mL sodium chloride solutions, is evaporated near dry, addition 2mLHCl, and re-evaporation is repeated 3 times, removed to closely doing,
Surface plate and wall of cup is washed with water, adds water to 100mL, in the case where being stirred continuously, 4mL hydrazine hydrate solutions are added dropwise, heating is boiled
30min, make golden coagulative precipitation, remove, be cooled to room temperature；
(2) test solution is filtered in 400mL beakers with middling speed quantitative filter paper, rinses surface plate, beaker, filter paper with water and sink
Form sediment 4~6 times, residue is used for the recovery of gold；
(3) 5mL sulfuric acid is added in filtrate, is heated to emitting dense white cigarette, removes surface plate, continue to be heated to wet salt shape, remove,
Cooling；
(4) 20mL sulfuric acid is added, cap upper surface ware, dissolves by heating salt, it is slightly cold, surface plate and wall of cup are purged with water, and
Volume is diluted to 100mL；
(5) 2~3g ammonium chlorides are added, are dissolved by heating, remove slightly cold, add 15~20mL ammoniacal liquor, beaker is placed in 60~
30min is heated in 70 DEG C of water-baths, is removed, the dimethylglyoxime solution of 10mL 2% is added by every 20mg nickel, fully shakes, stand
30min, filtered with middling speed quantitative filter paper, with ammonia scrubbing precipitation and each 5 times of beaker；
(6) precipitation is put back into former beaker together with filter paper, is precipitated with 20mL dissolving with hydrochloric acid, add water to 100mL, added
20mL EDTA standard titration solutions, 20mL hexamethylenetetramine solution is added, 2 drop xylenol orange solution, solution is adjusted with ammoniacal liquor
To pH=6, titrated with zinc chloride standard titration solution, 20mL hexamethylenetetramine solution is added when closing on terminal, uses zinc chloride
Standard titration solution is titrated to solution and is changed into the purplish red content for being terminal, calculating nickel from yellow；
(7) full procedure blank is done in company with sample.
In step (1) of the present invention, it is 3 volume hydrochloric acid and 1 volume nitric acid mixed preparing to add wang aqueous solution；Sodium chloride
Concentration is 100g/L, concentration of hydrazine hydrate 1+9.
In step (3) of the present invention, sulfuric acid concentration is 1+1.
In step (4) of the present invention, sulfuric acid concentration is 1+9.
In step (5) of the present invention, ammonia concn is 2+98.
In step (6) of the present invention, concentration of hydrochloric acid 1+2.
The configuration of EDTA standard titration solutions and scaling method are as follows in step (6) of the present invention：
The configuration of EDTA standard titration solutions：18g disodium ethylene diamine tetraacetates are weighed in 1000mL volumetric flasks, are added water to
Groove, shakes dissolving, and placement is stablized three days, shaken up before demarcation；
Zinc standard solution is prepared：2.0000g metallic zincs 99.99% accurately are weighed in 250mL beakers, add 20mL hydrochloric acid,
Concentration 1+1, table ware is covered, moved into after being heated to all dissolvings in 1000mL volumetric flasks, with water constant volume, this solution is respectively containing zinc
2.00mg/mL；
Demarcation：Four parts of the above-mentioned Zinc standard solutions of 10.00mL are pipetted, are respectively placed in 250mL beakers, addition 20mL acetic acid-
Sodium acetate buffer solution, add 100mL water, then add 2 drop 5g/L xylenol orange indicator, be titrated to EDTA standard titration solutions molten
Liquid makees blank test by aubergine to glassy yellow, as terminal, during demarcation；
The extreme difference of the volume of the EDTA standard titration solutions of four parts of Zinc standard solution consumption is no more than 0.1mL, otherwise again
Demarcation, the concentration of EDTA standard titration solutions is calculated by formula (1)：
In formula：
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
c0The mass concentration of-Zinc standard solution, unit are gram every milliliter (g/mL)；
v1- volume of Zinc standard solution is pipetted, unit is milliliter (mL)；
v2The volume (mL) of the EDTA standard titration solutions consumed during-titration sample；
Mole matter of the 0.06538-zinc suitable with 1mol/L EDTA standard titration solutions c (EDTA)=1.000mol/L
Amount, unit is gram every mole (g/mol).
In step (6) of the present invention, hexamethylenetetramine solution concentration 200g/L, xylenol orange solution concentration 5g/L,
Ammonia concn 1+1.
In step (6) of the present invention, the compound method and scaling method of zinc chloride standard titration solution are as follows：
Prepare：4.2g zinc chloride are weighed, moves into 1000mL volumetric flasks after adding a small amount of water dissolving, with water constant volume, shakes up；
Demarcation：4 parts of 20mL EDTA standard titration solutions are pipetted, add 20mL hexamethylenetetramine solution, concentration 200g/
L, 2 drop xylenol orange solution, concentration 5g/L, solution is adjusted to pH=6, ammonia concn 1+1 with ammoniacal liquor, with zinc chloride standardized titration
Solution is titrated, and 20mL hexamethylenetetramine solution is added when closing on terminal, concentration 200g/L, is dripped with zinc chloride standard titration solution
It is terminal to determine to be changed into purplish red from yellow to solution；The body of the EDTA standard titration solutions of four parts of zinc chloride standard titration solution consumption
Long-pending extreme difference is no more than 0.1mL, otherwise re-scales, and the concentration of zinc chloride standard titration solution is calculated by formula (2)：
In formula：
c1The concentration of-chlorination Zinc standard solution, unit are gram every milliliter (mol/L)；
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
v3- volumes of EDTA standard titration solutions is pipetted, unit is milliliter (mL)
v4The volume (mL) of zinc chloride is consumed during-titration sample.
In step (6) of the present invention, the calculation formula of nickel is as follows：
In formula：
WNiThe mass fraction of-nickel, %；
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
c1The concentration of-zinc chloride standard titration solution, unit are gram every milliliter (mol/L)；
V5The volume of-addition EDTA standard titration solutions, unit is milliliter (mL)；
V6The volume of zinc chloride standard titration solution is consumed during-titration, unit is milliliter (mL)；
m0- sample amount, unit are gram (g).
The present invention, with aqua regia dissolution sample, precipitates separation gold, filtering, filter residue is used for according to the property of thick gold with hydrazine hydrate
Recovery is golden, and ammonium chloride is added in filtrate and ammoniacal liquor forms alkaline buffer system, adds dimethylglyoxime precipitation and separates nickel, with six first
Urotropine is cushioning liquid, adds excessive EDTA and nickel reactant, and using xylenol orange as indicator, zinc chloride is excessive EDTA
It is terminal that titrant, which is titrated to solution to be changed into purplish red from yellow, calculates the content of nickel in thick gold.The present invention is suitable for thick gold
The measure of nickel content of the nickel content more than 5%.
Beneficial effects of the present invention：
(1) present invention has filled up the blank of nickel quantity measuring method in thick gold, and slightly the nickel content in gold is accurate to the measure of gold
Degree has a significant impact, can in the thick gold of Accurate Determining the amount of nickel be Accurate Determining gold content premise, and thick gold is currently without
The standard of the measure nickel of shaping, therefore the present invention has the function that to plug a gap.
(2) present invention completes the recovery of gold while nickel is determined, and gold is as element most valuable in thick gold, in sample
It is the recovery that complete gold after measure, the present invention completes the separation of gold in the early stage of measure nickel, and gold is in one easily
In the state of recovery, therefore the recovery for gold also there is provided easily method.
(3) mode and the mark-on reclaims of actual sample that the present invention prepares by using standard liquid, the method for checking
The degree of accuracy and precision, as a result either standard preparation sample or actual sample, its rate of recovery 99%~101% it
Between, standard preparation sample precision is respectively less than 0.1%, it is seen that nickel amount in thick gold of the Accurate Determining content of the present invention more than 5%, surveys
It is wide to determine scope, preci-sion and accuracy is good
(4) present invention is simple to operate, and the content of the invention includes acid dissolving and filtering, and simple complexometry, simple to operate,
And process is easily controlled, therefore it is adapted to batch detection.
Embodiment
Comprise the following steps：
(1) appropriate sample is weighed, is placed in 250mL beakers, adds 10mL chloroazotic acid, cap upper surface ware, low-temperature heat to examination
Sample is completely dissolved, addition 1mL sodium chloride solutions, is evaporated near dry, addition 2mLHCl, and re-evaporation is repeated 3 times, removed to closely doing,
Surface plate and wall of cup is washed with water, adds water to 100mL, in the case where being stirred continuously, 4mL hydrazine hydrate solutions are added dropwise, heating is boiled
30min, make golden coagulative precipitation, remove, be cooled to room temperature；
(2) test solution is filtered in 400mL beakers with middling speed quantitative filter paper, rinses surface plate, beaker, filter paper with water and sink
Form sediment 4~6 times, residue is used for the recovery of gold；
(3) 5mL sulfuric acid (1+1) is added in filtrate, is heated to emitting dense white cigarette, removes surface plate, continue to be heated to wet salt shape,
Remove, cool down；
(4) 20mL sulfuric acid (1+9) is added, cap upper surface ware, dissolves by heating salt, it is slightly cold, purge surface plate and cup with water
Wall, and volume is diluted to 100mL；
(5) 2~3g ammonium chlorides are added, are dissolved by heating, remove slightly cold, add 15~20mL ammoniacal liquor, beaker is placed in 60~
30min is heated in 70 DEG C of water-baths, is removed, the dimethylglyoxime solution of 10mL 2% is added by every 20mg nickel, fully shakes, stand
30min, filtered with middling speed quantitative filter paper, ammoniacal liquor (2+98) washing precipitation and each 5 times of beaker；
(6) precipitation is put back into former beaker together with filter paper, is dissolved and precipitated with 20mL hydrochloric acid (1+2), add water to 100mL,
20mL EDTA standard titration solutions are added, EDTA amount adds 20mL hexamethylenetetramine solution depending on the height of nickel content
(200g/L), 2 drop xylenol orange solution (5g/L), solution is adjusted to pH=6 with ammoniacal liquor (1+1), it is molten with zinc chloride standardized titration
Drop is determined, and 20mL hexamethylenetetramines solution (200g/L) is added when closing on terminal, is titrated to zinc chloride standard titration solution
Solution is changed into the purplish red content for being terminal, calculating nickel from yellow；
(7) full procedure blank is done in company with sample.
In step (1) of the present invention, it is 3 volume hydrochloric acid and 1 volume nitric acid mixed preparing to add wang aqueous solution；
All acid being related to of the present invention, except special instruction is the pure concentrated acid of analysis, sodium chloride concentration 100g/L, it is hydrated
Hydrazine concentration is (1+9)；
In step (2) of the present invention, washing times can not be less than 4 times, because washing filtrate will carry out nickel-silicon nitride, be washed
It is very few to wash number, might have nickel and remain in makes Lower result in beaker；
In step (5) of the present invention, the addition of dimethylglyoxime is not to be exceeded the 10% of reagent cumulative volume, otherwise fourth two
The solubility increase of ketoxime nickel, in addition, after precipitation solution should be made to be cooled to room temperature can filter, because the fourth two in the solution of heat
The solubility of ketoxime nickel can also increase；
The configuration of EDTA standard titration solutions and scaling method are as follows in step (6) of the present invention：
The configuration of EDTA standard titration solutions：18g disodium ethylene diamine tetraacetates are weighed in 1000mL volumetric flasks, are added water to
Groove, shakes dissolving, and placement is stablized three days, shaken up before demarcation；
Zinc standard solution is prepared：2.0000g metallic zincs (99.99%) accurately are weighed in 250mL beakers, add 20mL hydrochloric acid
(1+1), table ware is covered, moved into after being heated to all dissolvings in 1000mL volumetric flasks, with water constant volume, this solution is respectively containing zinc
2.00mg/mL；
Demarcation：Four parts of the above-mentioned Zinc standard solutions of 10.00mL are pipetted, are respectively placed in 250mL beakers, addition 20mL acetic acid-
Sodium acetate buffer solution, add 100mL water, then add 2 drop 5g/L xylenol orange indicator, be titrated to EDTA standard titration solutions molten
Liquid makees blank test by aubergine to glassy yellow, as terminal, during demarcation；
The extreme difference of the volume of the EDTA standard titration solutions of four parts of Zinc standard solution consumption is no more than 0.1mL, otherwise again
Demarcation, the concentration of EDTA standard titration solutions is calculated by formula (1)：
In formula：
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
c0The mass concentration of-Zinc standard solution, unit are gram every milliliter (g/mL)；
v1- volume of Zinc standard solution is pipetted, unit is milliliter (mL)；
v2The volume (mL) of the EDTA standard titration solutions consumed during-titration sample；
0.06538-with mole of the suitable zinc of 1mol/L EDTA standard titration solutions [c (EDTA)=1.000mol/L]
Quality, unit are gram every mole (g/mol).
In step (6) of the present invention, the compound method and scaling method of zinc chloride standard titration solution are as follows：
Prepare：4.2g zinc chloride are weighed, moves into 1000mL volumetric flasks after adding a small amount of water dissolving, with water constant volume, shakes up；
Demarcation：Pipette 4 parts of 20mL EDTA standard titration solutions, add 20mL hexamethylenetetramines solution (200g/L), 2
Xylenol orange solution (5g/L) is dripped, solution is adjusted to pH=6 with ammoniacal liquor (1+1), is titrated, closed on zinc chloride standard titration solution
20mL hexamethylenetetramines solution (200g/L) is added during terminal, be titrated to solution with zinc chloride standard titration solution is become by yellow
For it is purplish red be terminal；The extreme difference of the volume of the EDTA standard titration solutions of four parts of zinc chloride standard titration solution consumption is no more than
0.1mL, otherwise re-scale, the concentration of zinc chloride standard titration solution is calculated by formula (2)：
In formula：
c1The concentration of-chlorination Zinc standard solution, unit are gram every milliliter (mol/L)；
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
v3- volumes of EDTA standard titration solutions is pipetted, unit is milliliter (mL)
v4The volume (mL) of zinc chloride is consumed during-titration sample.
In step (6) of the present invention, the calculation formula of nickel is as follows：
In formula：
WNiThe mass fraction of-nickel, %；
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
c1The concentration of-zinc chloride standard titration solution, unit are gram every milliliter (mol/L)；
V5The volume of-addition EDTA standard titration solutions, unit is milliliter (mL)；
V6The volume of zinc chloride standard titration solution is consumed during-titration, unit is milliliter (mL)；
m0- sample amount, unit are gram (g).
The present invention is further illustrated by specific experiment example below.
Experimental example 1
A kind of mixed standard solution is configured, respectively containing golden 150mg, silver-colored 8.0mg, zinc 40mg, copper 250mg, nickel 40mg, 4 parts,
It is respectively placed in 250mL beakers, adds 10mL chloroazotic acid, cap upper surface ware.Low-temperature heat to sample is completely dissolved, and adds 1mL chlorine
Change sodium solution, be evaporated near dry.2mLHCL is added, re-evaporation is done near, is repeated 3 times, removes, surface plate and cup is washed with water
Wall, 100mL is added water to, in the case where being stirred continuously, 4mL hydrazine hydrate solutions are added dropwise, heating boils 30min, makes golden coagulative precipitation.Take
Under, it is cooled to room temperature.Test solution is filtered in 400mL beakers with middling speed quantitative filter paper, surface plate, beaker, filter paper are rinsed with water
And precipitate 4 times.Residue is used for the recovery of gold.It is about 20mL that filtrate, which is placed in heating evaporation to volume on electric furnace pan, adds 5mL sulphur
Acid, it is heated to emitting dense white cigarette, removes surface plate, continue to be heated to wet salt shape, remove, cools down.Add 20mL sulfuric acid, cap upper surface
Ware, salt is dissolved by heating, it is slightly cold, surface plate and wall of cup are purged with water, and dilute volume to 100mL or so.Add 2~3g chlorinations
Ammonium, dissolve by heating, remove it is slightly cold, add 15~20mL ammoniacal liquor, beaker is placed in 60~70 DEG C of water-baths and heats 30min, is removed,
10mL dimethylglyoxime solution is added, is fully shaken, stands 30min.Filtered with middling speed quantitative filter paper, ammoniacal liquor (2+98) washing precipitation
And each 5 times of beaker, precipitation is put back into former beaker together with filter paper, is dissolved and precipitated with 20mL hydrochloric acid (1+2), add water to 100mL,
20mL EDTA solution is added, 20mL hexamethylenetetramine solution is added, 2 drop xylenol orange solution, solution is adjusted to pH with ammoniacal liquor
=6, titrated with liquor zinci chloridi, 20mL hexamethylenetetramine solution added when closing on terminal, with zinc chloride be titrated to solution by
It is terminal that yellow, which is changed into purplish red, and the content for calculating nickel is respectively 39.80mg；39.78mg, 39.82mg, 39.80mg, now nickel return
Yield is 99.50%；Precision is 0.041%.
Experimental example 2
A kind of mixed standard solution is configured, respectively containing golden 300mg, silver-colored 8.0mg, zinc 12mg, copper 150mg, nickel 30mg, is placed in
In 250mL beakers, 10mL chloroazotic acid, cap upper surface ware are added.Low-temperature heat to sample is completely dissolved, and adds 1mL sodium chloride solutions,
It is evaporated near dry.2mLHCL is added, re-evaporation is done near, is repeated 3 times, removes, surface plate and wall of cup is washed with water, adds water to
100mL, in the case where being stirred continuously, 4mL hydrazine hydrate solutions are added dropwise, heating boils 30min, makes golden coagulative precipitation.Remove, be cooled to room
Temperature.Test solution is filtered in 400mL beakers with middling speed quantitative filter paper, surface plate, beaker, filter paper is rinsed with water and precipitates 4 times.It is residual
Slag is used for the recovery of gold.It is about 20mL that filtrate, which is placed in heating evaporation to volume on electric furnace pan, adds 5mL sulfuric acid, is heated to emitting dense
White cigarette, surface plate is removed, continue to be heated to wet salt shape, remove, cooled down.20mL sulfuric acid is added, cap upper surface ware, dissolves by heating salt
Class, it is slightly cold, surface plate and wall of cup are purged with water, and dilute volume to 100mL or so.2~3g ammonium chlorides are added, are dissolved by heating,
Remove slightly cold, add 15~20mL ammoniacal liquor, beaker is placed in 60~70 DEG C of water-baths and heats 30min, is removed, add 10mL fourths two
Ketoxime solution, fully shake, stand 30min.Filtered with middling speed quantitative filter paper, ammoniacal liquor (2+98) washing precipitation and each 5 times of beaker,
Precipitation is put back into former beaker together with filter paper, is dissolved and precipitated with 20mL hydrochloric acid (1+2), add water to 100mL, add 20mL
EDTA solution, 20mL hexamethylenetetramine solution is added, 2 drop xylenol orange solution, solution is adjusted to pH=6 with ammoniacal liquor, uses chlorine
Change zinc solution titration, 20mL hexamethylenetetramine solution is added when closing on terminal, be titrated to solution with zinc chloride is changed into from yellow
The purplish red content 29.98mg for being terminal, calculating nickel；29.96mg；29.93mg；29.95mg, now nickel recovery is 99.83%；
Precision is 0.069%
Embodiment 3
A unknown content slightly golden sample is determined, claims sample 0.5000g, is placed in 250mL beakers, 10mL chloroazotic acid is added, covers
Surface plate.Low-temperature heat to sample is completely dissolved, and adds 1mL sodium chloride solutions, is evaporated near dry.Add 2mLHCL, re-evaporation
Done near, be repeated 3 times, remove, surface plate and wall of cup is washed with water, adds water to 100mL, in the case where being stirred continuously, 4mL hydrations are added dropwise
Hydrazine solution, heating boil 30min, make golden coagulative precipitation.Remove, be cooled to room temperature.With middling speed quantitative filter paper by test solution filter in
In 400mL beakers, rinse surface plate, beaker, filter paper with water and precipitate 4 times.Residue is used for the recovery of gold.Filtrate is placed in electric furnace pan
Upper heating evaporation to volume is about 20mL, adds 5mL sulfuric acid, is heated to emitting dense white cigarette, removes surface plate, continue to be heated to wet salt
Shape, remove, cool down.20mL sulfuric acid is added, cap upper surface ware, dissolves by heating salt, it is slightly cold, surface plate and wall of cup are purged with water,
And volume is diluted to 100mL or so.Add 2~3g ammonium chlorides, dissolve by heating, remove it is slightly cold, add 15~20mL ammoniacal liquor, will burn
Cup, which is placed in 60~70 DEG C of water-baths, heats 30min, removes, and adds 10mL dimethylglyoxime solution, fully shakes, stands 30min.With
Middling speed quantitative filter paper filters, ammoniacal liquor (2+98) washing precipitation and each 5 times of beaker, and precipitation is put back into former beaker together with filter paper,
Dissolved and precipitated with 20mL hydrochloric acid (1+2), add water to 100mL, add 20mL EDTA solution, it is molten to add 20mL hexamethylenetetramines
Liquid, 2 drop xylenol orange solution, solution is adjusted to PH=6 with ammoniacal liquor, is titrated with liquor zinci chloridi, 20mL is added when closing on terminal
Hexamethylenetetramine solution, it is titrated to solution with zinc chloride and the purplish red content 7.85% for being terminal, calculating nickel is changed into from yellow.
Recovery of standard addition measure is carried out with herewith unknown sample according to the method described above, claims sample 0.5000g, mark-on amount is：Add
1mL 40mg/mL nickel standard liquids, the content for measuring nickel is 15.78%, and the recovery of standard addition for calculating nickel is 99.12%.
Embodiment 4
A unknown content slightly golden sample is determined, claims sample 0.5000g, is placed in 250mL beakers, 10mL chloroazotic acid is added, covers
Surface plate.Low-temperature heat to sample is completely dissolved, and adds 1mL sodium chloride solutions, is evaporated near dry.Add 2mLHCL, re-evaporation
Done near, be repeated 3 times, remove, surface plate and wall of cup is washed with water, adds water to 100mL, in the case where being stirred continuously, 4mL hydrations are added dropwise
Hydrazine solution, heating boil 30min, make golden coagulative precipitation.Remove, be cooled to room temperature.With middling speed quantitative filter paper by test solution filter in
In 400mL beakers, rinse surface plate, beaker, filter paper with water and precipitate 4 times.Residue is used for the recovery of gold.Filtrate is placed in electric furnace pan
Upper heating evaporation to volume is about 20mL, adds 5mL sulfuric acid, is heated to emitting dense white cigarette, removes surface plate, continue to be heated to wet salt
Shape, remove, cool down.20mL sulfuric acid is added, cap upper surface ware, dissolves by heating salt, it is slightly cold, surface plate and wall of cup are purged with water,
And volume is diluted to 100mL or so.Add 2~3g ammonium chlorides, dissolve by heating, remove it is slightly cold, add 15~20mL ammoniacal liquor, will burn
Cup, which is placed in 60~70 DEG C of water-baths, heats 30min, removes, and adds 10mL dimethylglyoxime solution, fully shakes, stands 30min.With
Middling speed quantitative filter paper filters, ammoniacal liquor (2+98) washing precipitation and each 5 times of beaker, and precipitation is put back into former beaker together with filter paper,
Dissolved and precipitated with 20mL hydrochloric acid (1+2), add water to 100mL, add 20mL EDTA solution, it is molten to add 20mL hexamethylenetetramines
Liquid, 2 drop xylenol orange solution, solution is adjusted to PH=6 with ammoniacal liquor, is titrated with liquor zinci chloridi, 20mL is added when closing on terminal
Hexamethylenetetramine solution, it is terminal to be titrated to solution to be changed into purplish red from yellow with zinc chloride, and full procedure blank is done in company with sample,
Calculate the content 10.50% of nickel.
Recovery of standard addition measure is carried out with herewith unknown sample according to the method described above, claims sample 0.5000g, mark-on amount is：Add
1mL, 50mg/mL nickel standard liquid, the content for measuring nickel is 20.58%, and the recovery of standard addition for calculating nickel is 100.80%.
Claims (10)
1. a kind of nickel-silicon nitride method in thick gold, it is characterised in that comprise the following steps：
(1) appropriate sample is weighed, is placed in 250mL beakers, adds 10mL chloroazotic acid, cap upper surface ware, low-temperature heat is complete to sample
Fully dissolved, addition 1mL sodium chloride solutions are evaporated near dry, addition 2mLHCl, and re-evaporation is repeated 3 times, removed, use water to closely doing
Washing surface ware and wall of cup, add water to 100mL, in the case where being stirred continuously, 4mL hydrazine hydrate solutions are added dropwise, heating is boiled 30min, made
Golden coagulative precipitation, is removed, and is cooled to room temperature；
(2) test solution is filtered in 400mL beakers with middling speed quantitative filter paper, surface plate, beaker, filter paper and precipitation 4 is rinsed with water
~6 times, residue is used for the recovery of gold；
(3) 5mL sulfuric acid is added in filtrate, is heated to emitting dense white cigarette, removes surface plate, continue to be heated to wet salt shape, remove, it is cold
But；
(4) 20mL sulfuric acid is added, cap upper surface ware, dissolves by heating salt, it is slightly cold, surface plate and wall of cup are purged with water, and dilute
Volume is to 100mL；
(5) add 2~3g ammonium chlorides, dissolve by heating, remove it is slightly cold, add 15~20mL ammoniacal liquor, beaker is placed in 60~70 DEG C
30min is heated in water-bath, is removed, the dimethylglyoxime solution of 10mL 2% is added by every 20mg nickel, fully shakes, stand 30min, use
Middling speed quantitative filter paper filters, with ammonia scrubbing precipitation and each 5 times of beaker；
(6) precipitation is put back into former beaker together with filter paper, precipitated with 20mL dissolving with hydrochloric acid, add water to 100mL, add 20mL
EDTA standard titration solutions, 20mL hexamethylenetetramine solution is added, 2 drop xylenol orange solution, solution is adjusted to pH with ammoniacal liquor
=6, titrated with zinc chloride standard titration solution, 20mL hexamethylenetetramine solution is added when closing on terminal, with zinc chloride standard
Volumetric soiutions are titrated to solution and are changed into the purplish red content for being terminal, calculating nickel from yellow；
(7) full procedure blank is done in company with sample.
2. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (1), add
Wang aqueous solution is 3 volume hydrochloric acid and 1 volume nitric acid mixed preparing；Sodium chloride concentration is 100g/L, concentration of hydrazine hydrate 1+9.
3. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (3), sulfuric acid
Concentration is 1+1.
4. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (4), sulfuric acid
Concentration is 1+9.
5. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (5), ammoniacal liquor
Concentration is 2+98.
6. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (6), hydrochloric acid
Concentration 1+2.
7. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that EDTA in the step (6)
The configuration of standard titration solution and scaling method are as follows：
The configuration of EDTA standard titration solutions：18g disodium ethylene diamine tetraacetates are weighed in 1000mL volumetric flasks, add water to quarter
Line, shakes dissolving, and placement is stablized three days, shaken up before demarcation；
Zinc standard solution is prepared：2.0000g metallic zincs 99.99% accurately are weighed in 250mL beakers, add 20mL hydrochloric acid, concentration 1
+ 1, table ware is covered, is moved into after being heated to all dissolvings in 1000mL volumetric flasks, with water constant volume, this solution is respectively containing zinc
2.00mg/mL；
Demarcation：Four parts of the above-mentioned Zinc standard solutions of 10.00mL are pipetted, are respectively placed in 250mL beakers, add 20mL acetic acid-acetic acid
Sodium cushioning liquid, adds 100mL water, then adds 2 drop 5g/L xylenol orange indicator, with EDTA standard titration solutions be titrated to solution by
Aubergine makees blank test to glassy yellow, as terminal, during demarcation；
The extreme difference of the volume of the EDTA standard titration solutions of four parts of Zinc standard solution consumption is no more than 0.1mL, otherwise re-scales,
The concentration of EDTA standard titration solutions is calculated by formula (1)：
<mrow>
<mi>c</mi>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>c</mi>
<mn>0</mn>
</msub>
<mo>&CenterDot;</mo>
<msub>
<mi>v</mi>
<mn>1</mn>
</msub>
</mrow>
<mrow>
<msub>
<mi>v</mi>
<mn>2</mn>
</msub>
<mo>&times;</mo>
<mn>0.06538</mn>
</mrow>
</mfrac>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>1</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula：
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
c0The mass concentration of-Zinc standard solution, unit are gram every milliliter (g/mL)；
v1- volume of Zinc standard solution is pipetted, unit is milliliter (mL)；
v2The volume (mL) of the EDTA standard titration solutions consumed during-titration sample；
The molal weight of the 0.06538-zinc suitable with 1mol/L EDTA standard titration solutions c (EDTA)=1.000mol/L,
Unit is gram every mole (g/mol).
8. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (6), six times
Tetramine solution concentration 200g/L, xylenol orange solution concentration 5g/L, ammonia concn 1+1.
9. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (6), chlorination
The compound method of zinc standard titration solution and scaling method are as follows：
Prepare：4.2g zinc chloride are weighed, moves into 1000mL volumetric flasks after adding a small amount of water dissolving, with water constant volume, shakes up；
Demarcation：4 parts of 20mL EDTA standard titration solutions are pipetted, add 20mL hexamethylenetetramine solution, concentration 200g/L, 2 drops
Xylenol orange solution, concentration 5g/L, solution is adjusted to pH=6, ammonia concn 1+1 with ammoniacal liquor, with zinc chloride standard titration solution
Titration, adds 20mL hexamethylenetetramine solution, concentration 200g/L, is titrated to zinc chloride standard titration solution when closing on terminal
It is terminal that solution is changed into purplish red from yellow；The volume of the EDTA standard titration solutions of four parts of zinc chloride standard titration solution consumption
Extreme difference is no more than 0.1mL, otherwise re-scales, and the concentration of zinc chloride standard titration solution is calculated by formula (2)：
<mrow>
<msub>
<mi>c</mi>
<mn>1</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<mi>c</mi>
<mo>&CenterDot;</mo>
<msub>
<mi>v</mi>
<mn>3</mn>
</msub>
</mrow>
<msub>
<mi>v</mi>
<mn>4</mn>
</msub>
</mfrac>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>2</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula：
c1The concentration of-chlorination Zinc standard solution, unit are gram every milliliter (mol/L)；
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
v3- volumes of EDTA standard titration solutions is pipetted, unit is milliliter (mL)
v4The volume (mL) of zinc chloride is consumed during-titration sample.
10. nickel-silicon nitride method in a kind of thick gold according to claim 1, it is characterised in that in the step (6), nickel
Calculation formula it is as follows：
<mrow>
<msub>
<mi>W</mi>
<mrow>
<mi>N</mi>
<mi>i</mi>
</mrow>
</msub>
<mrow>
<mo>(</mo>
<mi>%</mi>
<mo>)</mo>
</mrow>
<mo>=</mo>
<mfrac>
<mrow>
<mn>58.70</mn>
<mo>&times;</mo>
<mrow>
<mo>(</mo>
<msub>
<mi>cV</mi>
<mn>5</mn>
</msub>
<mo>-</mo>
<msub>
<mi>c</mi>
<mn>1</mn>
</msub>
<msub>
<mi>V</mi>
<mn>6</mn>
</msub>
<mo>)</mo>
</mrow>
</mrow>
<msub>
<mi>m</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>3</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula：
WNiThe mass fraction of-nickel, %；
The concentration of c-EDTA standard titration solutions, unit are mole every liter (mol/L)；
c1The concentration of-zinc chloride standard titration solution, unit are gram every milliliter (mol/L)；
V5The volume of-addition EDTA standard titration solutions, unit is milliliter (mL)；
V6The volume of zinc chloride standard titration solution is consumed during-titration, unit is milliliter (mL)；
m0- sample amount, unit are gram (g).
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| CN108872213A (en) * | 2018-05-08 | 2018-11-23 | 中国航发北京航空材料研究院 | A method of high content nickel element in measurement Au82Ni alloy |
| CN108918752A (en) * | 2018-07-06 | 2018-11-30 | 华友新能源科技（衢州）有限公司 | A kind of method of nickel, cobalt and manganese total amount in complexometric titration NCM material |
| CN108982749A (en) * | 2018-06-25 | 2018-12-11 | 河钢股份有限公司 | The method for measuring Main elements nickel and copper content in monel |
| CN110044878A (en) * | 2019-05-05 | 2019-07-23 | 冯均利 | The rapid assay methods of nickel hydroxide phase in a kind of thick nickel hydroxide material |
| CN110907593A (en) * | 2019-11-22 | 2020-03-24 | 西北矿冶研究院 | Chemical analysis method for determining nickel in nickel catalyst by changing complex anions |
| CN113049572A (en) * | 2021-04-02 | 2021-06-29 | 山东省计量科学研究院 | Method for accurately measuring gold content in gold ornament containing osmium iridium ruthenium alloy |
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|---|---|---|---|---|
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| CN108982749A (en) * | 2018-06-25 | 2018-12-11 | 河钢股份有限公司 | The method for measuring Main elements nickel and copper content in monel |
| CN108918752A (en) * | 2018-07-06 | 2018-11-30 | 华友新能源科技（衢州）有限公司 | A kind of method of nickel, cobalt and manganese total amount in complexometric titration NCM material |
| CN110044878A (en) * | 2019-05-05 | 2019-07-23 | 冯均利 | The rapid assay methods of nickel hydroxide phase in a kind of thick nickel hydroxide material |
| CN110907593A (en) * | 2019-11-22 | 2020-03-24 | 西北矿冶研究院 | Chemical analysis method for determining nickel in nickel catalyst by changing complex anions |
| CN113049572A (en) * | 2021-04-02 | 2021-06-29 | 山东省计量科学研究院 | Method for accurately measuring gold content in gold ornament containing osmium iridium ruthenium alloy |
| CN113049572B (en) * | 2021-04-02 | 2023-02-28 | 山东省计量科学研究院 | Method for accurately measuring gold content in gold jewelry containing osmium-iridium-ruthenium alloy |
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