CN109387450A - Platinum content measuring method in a kind of platinum-nickel alloys ornaments - Google Patents
Platinum content measuring method in a kind of platinum-nickel alloys ornaments Download PDFInfo
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- CN109387450A CN109387450A CN201710672315.4A CN201710672315A CN109387450A CN 109387450 A CN109387450 A CN 109387450A CN 201710672315 A CN201710672315 A CN 201710672315A CN 109387450 A CN109387450 A CN 109387450A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/02—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation
Abstract
The invention discloses platinum content measuring methods in a kind of platinum-nickel alloys ornaments, comprising the following steps: (1) sample pretreatment；(2) claim sample dissolution；(3) degradation nitric acid；(4) complex acid is dissolved；(5) oxydrolysis；(6) rough segmentation platinum palladium component；(7) dissolution palladium precipitates hydrate；(8) hydrolysis is reoxidized；(9) second of separating platinum palladium component；(10) degradation sodium bromate；(11) ammonium chloroplatinate precipitate is generated；(12) diafiltration ammonium chloroplatinate precipitate；(13) diafiltration ammonium chloroplatinate precipitate.(14) ammonium chloroplatinate precipitate is dried；(15) ammonium chloroplatinate precipitate quality is calculated.The present invention improves and optimizes the chemical reaction condition and operating process that platinum cycling of elements is ammonium chloroplatinate precipitate, accuracy, stability, the reliability of measurement result are good, eliminate ammonium chloroplatinate pyrolytic and colorimetric or spectrometry procedure, shorten analytical cycle, analysis efficiency is improved, meets enterprise's production and quality controls needs.
Description
Technical field
The present invention relates to detection technique fields, more particularly, to platinum content measuring method in a kind of platinum-nickel alloys ornaments.
Background technique
Ammonium chloroplatinate gravimetric method is the main method of current domestic Quantitative Analysis of Pt Pd ornaments platinum content.Its principle
Be: the platinum element in platinum-nickel alloys sample is converted ammonium chloroplatinate precipitate by the after chemical reaction in water phase.Pass through height again
Temperature reaction, converts simple substance platinum for ammonium chloroplatinate.Simple substance platinum quality is weighed, most of platinum content in sample is calculated.Use chlorination
Stannous colorimetric method or spectra methods, measurement remain the platinum content in water phase.Two parts platinum amount is added to get platinum-nickel alloys sample
In platinum magnitude.It is, in principle, that two methods of this combinatorial chemistry and physics measure the ammonium chloroplatinate weight of sample platinum content
Method is not proper gravimetry.It in actual operation, it is long that there is analytical cycles, and equipment investment is big, easily
The deficiencies of generating accumulated error.
How to make ammonium chloroplatinate gravimetric method become it is simple, reliable and quick, with improve platinum-nickel alloys ornaments production efficiency and
Control of product quality efficiency is the direction that platinum ornaments production industry chemical analysis worker makes great efforts for many years.
Summary of the invention
It is good that goal of the invention of the invention is to provide for a kind of accuracy, stability, reliability, eliminates ammonium chloroplatinate
Pyrolytic and colorimetric or spectrometry procedure, shorten analytical cycle, improve platinum in the platinum-nickel alloys ornaments of analysis efficiency
Content assaying method.
To achieve the goals above, the invention adopts the following technical scheme:
Platinum content measuring method in a kind of platinum-nickel alloys ornaments of the invention, comprising the following steps:
(1) sample pretreatment: after platinum-nickel alloys sample is thinly sliced, obtaining platinum-nickel alloys sample blocks after being cut into small pieces, to
With.
(2) claim sample dissolution: in draught cupboard, weighing 0.3g platinum-nickel alloys sample blocks, and be denoted as m, be added in conical flask, point
Not Jia Ru the hydrochloric acid of 5ml mass fraction 0.36~0.38% and the nitric acid of 1ml mass fraction 0.65~0.68%, conical flask is set
In being heated on gas furnace, during heating, be added repeatedly into conical flask 5ml mass fraction 0.36~0.38% hydrochloric acid and
The nitric acid of 1ml mass fraction 0.65~0.68%, until platinum-nickel alloys sample blocks are completely dissolved.
(3) degradation nitric acid: continuing heating conical flask thermally decomposes remaining nitric acid, when solution is closely dry slowly into conical flask
The concentrated hydrochloric acid for adding 3ml mass fraction 36~38% continues to heat, and repeats to add the dense salt of 3ml mass fraction 36~38%
Acid, up to no Brown gas generates.Be heated to not can be heated to when solution is closely dry it is dry, to prevent insoluble black PtO2It generates, adds
NO is had at once after entering concentrated hydrochloric acid2Brown gas generates, must anti-bumping.
(4) it dissolves complex acid: adding the hydrochloric acid souring soln of 2ml mass fraction 0.36~0.38% into conical flask, then use
Wash bottle is added 7~8ml of distilled water, obtains complexing aqueous acid to elute in a manner of inner wall solid-state precipitate.Directly add water in the present invention
Excessively, helvolus infusible precipitate can be generated, therefore amount of water need to be controlled.
(5) oxydrolysis: the sodium hydroxide solution of mass fraction 20% is slowly added dropwise to nearly boiling in heating complexing aqueous acid
There is precipitating to generate to solution, the bromic acid sodium solution of 3ml mass fraction 10% is then added dropwise, continues heating and keep solution slightly boiled
Then sodium hydroxide solution and the 2ml mass fraction of 1ml mass fraction 10% is added dropwise respectively as 10% bromic acid sodium solution in 5min
Continuing heating makes solution slightly boiled 5 minutes, and adjusts pH value of solution to 8 ± 5, and the sodium bromate that 2ml mass fraction is 10% is added again
Solution simultaneously continues to heat slightly boiled solution 5min, finally by the quick water cooling of solution to 15 DEG C hereinafter, static suspension 5min.By solution
Quick water cooling is to 15 DEG C hereinafter, high price platinum is prevented to be reduced into low price platinum and palladium hydrate dissolution.
(6) sand core funnel and, connection suction filter pump, by solution step (5) in closely sealed with bottle,suction rough segmentation platinum palladium component: are taken
Sand core funnel is poured into, suction filter pump is opened and filters, purged conical flask inner wall 3 times with wash bottle, and cleaning solution is all moved to sand core leakage
Bucket filters, when in funnel precipitating filtered to it is close dry when, with wash bottle purging inner wall of hopper 3~4 times, make to be adsorbed in inner wall of hopper
Precipitating is all collected on funnel sand core filter plate, is finally drained precipitating, is obtained high concentration cl sodium platinate filtrate；
(7) dissolution palladium precipitates hydrate: separately a bottle,suction is taken, by there are the sand core funnel of precipitating and pumpings in step (6)
Filter flask is closely sealed, connects suction filter pump, and the concentrated hydrochloric acid of 1ml mass fraction 36~38% is added in sand core funnel, makes precipitating in funnel
All dissolutions purge inner wall of hopper with wash bottle, and by the precipitating for being adsorbed in inner wall, all purging is dissolved into acid solution in funnel, filter
And purged inner wall of hopper 3 times with wash bottle, make in funnel not residual palladium solution, obtains maroon solution；
(8) it reoxidizes hydrolysis: resulting maroon solution being checked the number and is all moved into former conical flask, is placed on gas furnace
The bromic acid sodium solution of 4~5ml mass fraction 10% is added in heating, and when bubble-free in solution generates, mass fraction 5% is added dropwise
Sodium bicarbonate solution, adjust pH value of solution to 8 ± 5, palladium made to be completely converted into dark brown precipitating and static solution 5min.It is added 4
The bromic acid sodium solution of~5ml mass fraction 10% is to aoxidize low price platinum compounds that may be present.
(9) second of separating platinum palladium component: separately taking a bottle,suction, sand core funnel is closely sealed therewith, suction filter pump in connection,
Solution in step (8) is poured into sand core funnel, suction filter pump is opened and filters, purged conical flask inner wall 3 times with wash bottle, and will washing
Liquid all moves to sand core funnel suction filtration, when in funnel precipitating filtered to it is close dry when, with wash bottle purging inner wall of hopper 3~4 times, make
The precipitating for being adsorbed in inner wall of hopper is all collected on funnel sand core filter plate, finally drains precipitating, obtains the filter of low-level chlorinated sodium platinate
Liquid；
(10) degradation sodium bromate: low-level chlorinated sodium platinate filtrate, which is moved in conical flask, to be placed in heat on natural gas furnace makes
Its is slightly boiled, be added 3~4ml mass fraction 36~38% concentrated hydrochloric acid, be heated to solution and be concentrated by evaporation to 5ml, in three times plus
Enter the high concentration cl sodium platinate filtrate in step (6), often plus a high concentration cl sodium platinate filtrate, adds 3~4ml mass fraction
36~38% concentrated hydrochloric acid is simultaneously close dry by solution heating, until solution heating is close dry.Addition 3~4ml mass fraction 36~
Solution can be made to become yellow green because sodium bromate decomposes generation free bromine (really bromic acid decomposition) after 38% concentrated hydrochloric acid.
(11) it generates ammonium chloroplatinate precipitate: the dense of 2ml mass fraction 36~38% being added into the conical flask of step (10)
Hydrochloric acid and 10ml distilled water make to precipitate whole dissolutions, then solution is fully transferred in beaker, and heating beaker is warming up to solution
80 DEG C, 5min is kept the temperature after agitating solution and points of 4~5 times additions 20g solid ammonium chlorides generation yellow ammonium chloroplatinate precipitates, by solution
Quick water cooling stands 10min after cooling to room temperature.By the quick water cooling of solution to room temperature, it would be possible to existing insoluble chlorine palladium acid
Ammonium is converted into soluble sub- ammonium chloropalladate.Occurs yolk yellow aggregation shape chloroplatinic acid ammonia-sinking immediately in solution after addition solid ammonium chloride
It forms sediment；By the quick water cooling of solution to room temperature, it is understood that there may be insoluble ammonium chloropalladate be converted into soluble sub- ammonium chloropalladate.
(12) diafiltration ammonium chloroplatinate precipitate: sand core crucible is placed in a beaker, and carefully pours into potassium bichromate concentrated sulfuric acid solution
To submergence crucible, sand core crucible is taken out after impregnating 30min, washes away washing lotion with tap water, distilled water elutes the inside and outside wall of sand core crucible
Sand core crucible is placed on bottle,suction afterwards, suction filter pump is connected, distilled water is added in sand core crucible, cleans crucible with the mode of suction filtration
Sand core, clean sand core crucible are put into baking oven, under the conditions of 80 DEG C after constant temperature drying 1h, take out and are immediately placed in drier,
It is cooled to room temperature, weighs sand core crucible net weight after cooling with assay balance, record weight W1；Sand core crucible is close with bottle,suction
It closes, yellow ammonium chloroplatinate precipitate in conical flask is fully transferred in sand core crucible, is adsorbed in conical flask by suction filter pump in connection
The ammonium chloroplatinate precipitate of wall all washes sand core crucible with saturated ammonium chloride solution, filters, and collects colorless filtrate；
(13) under suction filtration state, the chlorine of ammonium chloroplatinate precipitate absorption diafiltration ammonium chloroplatinate precipitate: is washed away with dehydrated alcohol
Change ammonium saturated solution.Wash away the ammonium chloride saturated solution of sand core crucible inside and outside wall absorption completely with dehydrated alcohol.
(14) ammonium chloroplatinate precipitate is dried: by there are the sand core crucibles of ammonium chloroplatinate precipitate to be put into beaker, cap upper surface
Ware puts baking oven into, and under the conditions of 90 DEG C, constant temperature drying 60min quickly removes beaker, put into cold in drier after completing drying
But to room temperature；
(15) it calculates ammonium chloroplatinate precipitate quality: weighing ammonium chloroplatinate precipitate and sand core crucible gross mass with assay balance
W2, then subtract sand core crucible net weight W1To get ammonium chloroplatinate mass M, according to formula: platinum content percentage value Pt%=in sample
(w2-w1Platinum content percentage value in sample can be calculated in m × 100 ÷ of) × 195/444, in: W1For sand core crucible net weight, W2
For ammonium chloroplatinate precipitate and sand core crucible gross mass, m is sample quality, i.e. 0.3g.
Preferably, in step (1), sheet thickness 0.2mm.
Preferably, in step (1), platinum-nickel alloys sample blocks area < 1mm2。
Therefore, the invention has the following beneficial effects: by the further combing to platinum, palladium difference compound state property, change
Into with optimize the chemical reaction condition and operating process that platinum cycling of elements is ammonium chloroplatinate precipitate, it is dry to eliminate compound state palladium
It disturbs, ammonium chloroplatinate is made sufficiently to generate and precipitate, by directly weighing ammonium chloroplatinate quality and Chemical Calculation, obtain sample platinum content
As a result, accuracy, stability, reliability are good, ammonium chloroplatinate pyrolytic and colorimetric or spectrometry procedure are eliminated, is shortened
Analytical cycle, improves analysis efficiency, meets enterprise's production and quality controls needs.
Specific embodiment
Below by specific embodiment, the present invention will be further described.
Sample detected is made by the following method in following embodiments: accurately weighing 14.250X grams with assay balance
With each portion of 13.500X grams of high-purity platinum, then 0.750X grams and each portion of 1.500X grams of High Purity Palladium are accurately weighed, respectively will
14.250X grams of platinum and 0.750X grams of palladium are mixed into one group, and 13.500X grams of platinum and 1.500X grams of palladium are mixed into another group.By two groups
The platinum palladium mixture of different component ratio is respectively put into the graphite corundum crucibles of 2 different numbers, with mid-frequency melting furnace,
In 1850 DEG C of argon atmosphere, it is smelted into uniform Pt950Pd50 (platinum mass fraction 950 ‰) and Pt900Pd100 (platinum
‰) the alloy of mass fraction 900.(note: the platinum-nickel alloys block that first time melting obtains need to be divided into 1mm2The little particle of left and right,
It is placed again into graphite corundum crucible, with mid-frequency melting furnace with the same terms melting again.It so repeats secondary to get uniform platinum
Palldium alloy).
Embodiment 1
(1) sample pretreatment: by platinum-nickel alloys sample (Pt950Pd50, platinum mass fraction 950 ‰) be cut into a thickness of
After the thin slice of 0.2mm, it is cut into area < 1mm2Fritter after platinum-nickel alloys sample blocks, for use；
(2) claim sample dissolution: in draught cupboard, weighing 0.3g platinum-nickel alloys sample blocks, and be denoted as m, be added in conical flask, point
Not Jia Ru the hydrochloric acid of 5ml mass fraction 0.36% and the nitric acid of 1ml mass fraction 0.65%, conical flask is placed on gas furnace
During heating, the hydrochloric acid and 1ml mass fraction 0.65% of 5ml mass fraction 0.36% are added into conical flask repeatedly for heating
Nitric acid, until platinum-nickel alloys sample blocks are completely dissolved；
(3) degradation nitric acid: continuing heating conical flask thermally decomposes remaining nitric acid, when solution is closely dry slowly into conical flask
The concentrated hydrochloric acid for adding 3ml mass fraction 36% continues to heat, and repeats to add the concentrated hydrochloric acid of 3ml mass fraction 36%, until nothing
Brown gas generates；
(4) it dissolves complex acid: adding the hydrochloric acid souring soln of 2ml mass fraction 0.36~0.38% into conical flask, then use
Wash bottle is added 7~8ml of distilled water, obtains complexing aqueous acid to elute in a manner of inner wall solid-state precipitate；
(5) oxydrolysis: the sodium hydroxide solution of mass fraction 20% is slowly added dropwise to nearly boiling in heating complexing aqueous acid
There is precipitating to generate to solution, the bromic acid sodium solution of 3ml mass fraction 10% is then added dropwise, continues heating and keep solution slightly boiled
Then sodium hydroxide solution and the 2ml mass fraction of 1ml mass fraction 10% is added dropwise respectively as 10% bromic acid sodium solution in 5min
Continuing heating makes solution slightly boiled 5 minutes, and adjusts pH value of solution to 8 ± 5, and the sodium bromate that 2ml mass fraction is 10% is added again
Solution simultaneously continues to heat slightly boiled solution 5min, finally by the quick water cooling of solution to 15 DEG C hereinafter, static suspension 5min；
(6) sand core funnel and, connection suction filter pump, by solution step (5) in closely sealed with bottle,suction rough segmentation platinum palladium component: are taken
Sand core funnel is poured into, suction filter pump is opened and filters, purged conical flask inner wall 3 times with wash bottle, and cleaning solution is all moved to sand core leakage
Bucket filters, when in funnel precipitating filtered to it is close dry when, purged inner wall of hopper 3 times with wash bottle, make to be adsorbed in sinking for inner wall of hopper
It forms sediment and is all collected on funnel sand core filter plate, finally drain precipitating, obtain high concentration cl sodium platinate filtrate；
(7) dissolution palladium precipitates hydrate: separately a bottle,suction is taken, by there are the sand core funnel of precipitating and pumpings in step (6)
Filter flask is closely sealed, connects suction filter pump, and the concentrated hydrochloric acid of 1ml mass fraction 36% is added in sand core funnel, keeps precipitating in funnel whole
Dissolution purges inner wall of hopper with wash bottle, and by the precipitating for being adsorbed in inner wall, all purging is dissolved into acid solution in funnel, and suction filtration is used in combination
Wash bottle purges inner wall of hopper 3 times, makes in funnel not residual palladium solution, obtains maroon solution；
(8) it reoxidizes hydrolysis: resulting maroon solution being checked the number and is all moved into former conical flask, is placed on gas furnace
The bromic acid sodium solution of 4ml mass fraction 10% is added in heating, and when bubble-free in solution generates, the carbon of mass fraction 5% is added dropwise
Sour hydrogen sodium solution adjusts pH value of solution to 8 ± 5, palladium is made to be completely converted into dark brown precipitating and static solution 5min；
(9) second of separating platinum palladium component: separately taking a bottle,suction, sand core funnel is closely sealed therewith, suction filter pump in connection,
Solution in step (8) is poured into sand core funnel, suction filter pump is opened and filters, purged conical flask inner wall 3 times with wash bottle, and will washing
Liquid all moves to sand core funnel suction filtration, when in funnel precipitating filtered to it is close dry when, with wash bottle purging inner wall of hopper 3 times, make to inhale
The precipitating for investing inner wall of hopper is all collected on funnel sand core filter plate, finally drains precipitating, obtains low-level chlorinated sodium platinate filtrate；
(10) degradation sodium bromate: low-level chlorinated sodium platinate filtrate, which is moved in conical flask, to be placed in heat on natural gas furnace makes
Its is slightly boiled, and the concentrated hydrochloric acid of 4ml mass fraction 36% is added, is heated to solution and is concentrated by evaporation to 5ml, step is added in three times
(6) the high concentration cl sodium platinate filtrate in often plus a high concentration cl sodium platinate filtrate adds the dense of 4ml mass fraction 38%
Hydrochloric acid is simultaneously close dry by solution heating, until solution heating is close dry；
(11) it generates ammonium chloroplatinate precipitate: the concentrated hydrochloric acid of 2ml mass fraction 36% being added into the conical flask of step (10)
Making to precipitate whole dissolutions with 10ml distilled water, then solution is fully transferred in beaker, heating beaker makes solution be warming up to 80 DEG C,
Agitating solution and point 4 addition 20g solid ammonium chlorides keep the temperature 5min after generating yellow ammonium chloroplatinate precipitate, by the quick water cooling of solution
To room temperature, 10min is stood after cooling；
(12) diafiltration ammonium chloroplatinate precipitate: sand core crucible is placed in a beaker, and carefully pours into potassium bichromate concentrated sulfuric acid solution
To submergence crucible, sand core crucible is taken out after impregnating 30min, washes away washing lotion with tap water, distilled water elutes the inside and outside wall of sand core crucible
Sand core crucible is placed on bottle,suction afterwards, suction filter pump is connected, distilled water is added in sand core crucible, cleans crucible with the mode of suction filtration
Sand core, clean sand core crucible are put into baking oven, under the conditions of 80 DEG C after constant temperature drying 1h, take out and are immediately placed in drier,
It is cooled to room temperature, weighs sand core crucible net weight after cooling with assay balance, record weight W1；Sand core crucible is close with bottle,suction
It closes, yellow ammonium chloroplatinate precipitate in conical flask is fully transferred in sand core crucible, is adsorbed in conical flask by suction filter pump in connection
The ammonium chloroplatinate precipitate of wall all washes sand core crucible with saturated ammonium chloride solution, filters, and collects colorless filtrate；
(13) under suction filtration state, the chlorine of ammonium chloroplatinate precipitate absorption diafiltration ammonium chloroplatinate precipitate: is washed away with dehydrated alcohol
Change ammonium saturated solution；
(14) ammonium chloroplatinate precipitate is dried: by there are the sand core crucibles of ammonium chloroplatinate precipitate to be put into beaker, cap upper surface
Ware puts baking oven into, and under the conditions of 90 DEG C, constant temperature drying 60min quickly removes beaker, put into cold in drier after completing drying
But to room temperature；
(15) it calculates ammonium chloroplatinate precipitate quality: weighing ammonium chloroplatinate precipitate and sand core crucible gross mass with assay balance
W2, then subtract sand core crucible net weight W1To get ammonium chloroplatinate mass M, according to formula: platinum content percentage value Pt%=in sample
(w2-w1Platinum content percentage value in sample can be calculated in m × 100 ÷ of) × 195/444, in: W1For sand core crucible net weight, W2
For ammonium chloroplatinate precipitate and sand core crucible gross mass, m is sample quality, i.e. 0.3g.
In addition taking 19 parts of 0.3g platinum-nickel alloys sample blocks again, (‰) Pt950Pd50, platinum mass fraction 950, repeat embodiment 1
After middle step, 20 parts of samples (Pt950Pd50, the arithmetic mean of instantaneous value of the platinum content percentage value of platinum mass fraction 950 ‰) are calculatedAnd platinum analysis standard deviationWherein,For the arithmetic average of sample platinum content percentage value
Value,
XiFor sample serial number,
diFor i sample platinum content percentage value absolute deviation,
S is standard deviation, and n is total number of samples.
Calculated result is as shown in table 1.
1 Pt950Pd50 sample analysis result of table
Embodiment 2
(1) sample pretreatment: by platinum-nickel alloys sample (Pt900Pd100, platinum mass fraction 900 ‰) be cut into a thickness of
After the thin slice of 0.2mm, it is cut into area < 1mm2Fritter after platinum-nickel alloys sample blocks, for use；
(2) claim sample dissolution: in draught cupboard, weighing 0.3g platinum-nickel alloys sample blocks, and be denoted as m, be added in conical flask, point
Not Jia Ru the hydrochloric acid of 5ml mass fraction 0.38% and the nitric acid of 1ml mass fraction 0.68%, conical flask is placed on gas furnace
During heating, the hydrochloric acid and 1ml mass fraction 0.68% of 5ml mass fraction 0.38% are added into conical flask repeatedly for heating
Nitric acid, until platinum-nickel alloys sample blocks are completely dissolved；
(3) degradation nitric acid: continuing heating conical flask thermally decomposes remaining nitric acid, when solution is closely dry slowly into conical flask
The concentrated hydrochloric acid for adding 3ml mass fraction 38% continues to heat, and repeats to add the concentrated hydrochloric acid of 3ml mass fraction 38%, until nothing
Brown gas generates；
(4) dissolve complex acid: into conical flask add 2ml mass fraction 0.38% hydrochloric acid souring soln, then with wash bottle with
Inner wall solid-state precipitate mode is eluted, 7~8ml of distilled water is added, obtains complexing aqueous acid；
(5) oxydrolysis: the sodium hydroxide solution of mass fraction 20% is slowly added dropwise to nearly boiling in heating complexing aqueous acid
There is precipitating to generate to solution, the bromic acid sodium solution of 3ml mass fraction 10% is then added dropwise, continues heating and keep solution slightly boiled
Then sodium hydroxide solution and the 2ml mass fraction of 1ml mass fraction 10% is added dropwise respectively as 10% bromic acid sodium solution in 5min
Continuing heating makes solution slightly boiled 5 minutes, and adjusts pH value of solution to 8 ± 5, and the sodium bromate that 2ml mass fraction is 10% is added again
Solution simultaneously continues to heat slightly boiled solution 5min, finally by the quick water cooling of solution to 15 DEG C hereinafter, static suspension 5min；
(6) sand core funnel and, connection suction filter pump, by solution step (5) in closely sealed with bottle,suction rough segmentation platinum palladium component: are taken
Sand core funnel is poured into, suction filter pump is opened and filters, purged conical flask inner wall 3 times with wash bottle, and cleaning solution is all moved to sand core leakage
Bucket filters, when in funnel precipitating filtered to it is close dry when, purged inner wall of hopper 4 times with wash bottle, make to be adsorbed in sinking for inner wall of hopper
It forms sediment and is all collected on funnel sand core filter plate, finally drain precipitating, obtain high concentration cl sodium platinate filtrate；
(7) dissolution palladium precipitates hydrate: separately a bottle,suction is taken, by there are the sand core funnel of precipitating and pumpings in step (6)
Filter flask is closely sealed, connects suction filter pump, and the concentrated hydrochloric acid of 1ml mass fraction 38% is added in sand core funnel, keeps precipitating in funnel whole
Dissolution purges inner wall of hopper with wash bottle, and by the precipitating for being adsorbed in inner wall, all purging is dissolved into acid solution in funnel, and suction filtration is used in combination
Wash bottle purges inner wall of hopper 3 times, makes in funnel not residual palladium solution, obtains maroon solution；
(8) it reoxidizes hydrolysis: resulting maroon solution being checked the number and is all moved into former conical flask, is placed on gas furnace
The bromic acid sodium solution of 5ml mass fraction 10% is added in heating, and when bubble-free in solution generates, the carbon of mass fraction 5% is added dropwise
Sour hydrogen sodium solution adjusts pH value of solution to 8 ± 5, palladium is made to be completely converted into dark brown precipitating and static solution 5min；
(9) second of separating platinum palladium component: separately taking a bottle,suction, sand core funnel is closely sealed therewith, suction filter pump in connection,
Solution in step (8) is poured into sand core funnel, suction filter pump is opened and filters, purged conical flask inner wall 3 times with wash bottle, and will washing
Liquid all moves to sand core funnel suction filtration, when in funnel precipitating filtered to it is close dry when, with wash bottle purging inner wall of hopper 3~4 times, make
The precipitating for being adsorbed in inner wall of hopper is all collected on funnel sand core filter plate, finally drains precipitating, obtains the filter of low-level chlorinated sodium platinate
Liquid；
(10) degradation sodium bromate: low-level chlorinated sodium platinate filtrate, which is moved in conical flask, to be placed in heat on natural gas furnace makes
Its is slightly boiled, and the concentrated hydrochloric acid of 3ml mass fraction 38% is added, is heated to solution and is concentrated by evaporation to 5ml, step is added in three times
(6) the high concentration cl sodium platinate filtrate in often plus a high concentration cl sodium platinate filtrate adds the dense of 3ml mass fraction 38%
Hydrochloric acid is simultaneously close dry by solution heating, until solution heating is close dry；
(11) it generates ammonium chloroplatinate precipitate: the concentrated hydrochloric acid of 2ml mass fraction 38% being added into the conical flask of step (10)
Making to precipitate whole dissolutions with 10ml distilled water, then solution is fully transferred in beaker, heating beaker makes solution be warming up to 80 DEG C,
Agitating solution and point 5 addition 20g solid ammonium chlorides keep the temperature 5min after generating yellow ammonium chloroplatinate precipitate, by the quick water cooling of solution
To room temperature, 10min is stood after cooling；
(12) diafiltration ammonium chloroplatinate precipitate: sand core crucible is placed in a beaker, and carefully pours into potassium bichromate concentrated sulfuric acid solution
To submergence crucible, sand core crucible is taken out after impregnating 30min, washes away washing lotion with tap water, distilled water elutes the inside and outside wall of sand core crucible
Sand core crucible is placed on bottle,suction afterwards, suction filter pump is connected, distilled water is added in sand core crucible, cleans crucible with the mode of suction filtration
Sand core, clean sand core crucible are put into baking oven, under the conditions of 80 DEG C after constant temperature drying 1h, take out and are immediately placed in drier,
It is cooled to room temperature, weighs sand core crucible net weight after cooling with assay balance, record weight W1；Sand core crucible is close with bottle,suction
It closes, yellow ammonium chloroplatinate precipitate in conical flask is fully transferred in sand core crucible, is adsorbed in conical flask by suction filter pump in connection
The ammonium chloroplatinate precipitate of wall all washes sand core crucible with saturated ammonium chloride solution, filters, and collects colorless filtrate；
(13) under suction filtration state, the chlorine of ammonium chloroplatinate precipitate absorption diafiltration ammonium chloroplatinate precipitate: is washed away with dehydrated alcohol
Change ammonium saturated solution；
(14) ammonium chloroplatinate precipitate is dried: by there are the sand core crucibles of ammonium chloroplatinate precipitate to be put into beaker, cap upper surface
Ware puts baking oven into, and under the conditions of 90 DEG C, constant temperature drying 60min quickly removes beaker, put into cold in drier after completing drying
But to room temperature；
(15) it calculates ammonium chloroplatinate precipitate quality: weighing ammonium chloroplatinate precipitate and sand core crucible gross mass with assay balance
W2, then subtract sand core crucible net weight W1To get ammonium chloroplatinate mass M, according to formula: platinum content percentage value Pt%=in sample
(w2-w1Platinum content percentage value in sample can be calculated in m × 100 ÷ of) × 195/444, in: W1For sand core crucible net weight, W2
For ammonium chloroplatinate precipitate and sand core crucible gross mass, m is sample quality, i.e. 0.3g.
In addition taking 19 parts of 0.3g platinum-nickel alloys sample blocks again, (‰) Pt900Pd100, platinum mass fraction 900, repeat embodiment
In 1 after step, 20 parts of samples (Pt900Pd100, the arithmetic mean of instantaneous value of the platinum content percentage value of platinum mass fraction 900 ‰) are calculatedAnd platinum analysis standard deviationWherein,For the arithmetic average of sample platinum content percentage value
Value,
XiFor sample serial number,
diFor i sample platinum content percentage value absolute deviation,
S is standard deviation, and n is total number of samples.
Calculated result is as shown in table 2.
2 Pt900Pd100 sample analysis result of table
Precision, the accuracy that can be seen that testing result of the invention from table 1, table 2 are good, meet conventional weight analysis
It is required that.
Platinum content measuring method accuracy, stability, reliability are good in platinum-nickel alloys ornaments of the invention, are not necessarily to chlorine platinum
Sour ammonium pyrolytic and colorimetric or spectrometry procedure, enormously simplify analytic process, shorten analytical cycle (analysis time by
It shorten within 2 days 1 day), analysis cost is reduced, analysis efficiency is improved, meets enterprise's production and quality controls needs.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (3)
1. platinum content measuring method in a kind of platinum-nickel alloys ornaments, which comprises the following steps:
(1) sample pretreatment: after platinum-nickel alloys sample is thinly sliced, platinum-nickel alloys sample blocks are obtained after being cut into small pieces, for use；
(2) claim sample dissolution: in draught cupboard, weigh 0.3g platinum-nickel alloys sample blocks, and be denoted as m, be added conical flask in, respectively plus
Enter the hydrochloric acid of 5ml mass fraction 0.36~0.38% and the nitric acid of 1ml mass fraction 0.65~0.68%, conical flask is placed in day
It is heated on right steam stove, during heating, the hydrochloric acid and 1ml matter of 5ml mass fraction 0.36~0.38% is added repeatedly into conical flask
The nitric acid of score 0.65~0.68% is measured, until platinum-nickel alloys sample blocks are completely dissolved；
(3) degradation nitric acid: continuing heating conical flask thermally decomposes remaining nitric acid, slowly adds when solution is closely dry into conical flask
The concentrated hydrochloric acid of 3ml mass fraction 36~38% continues to heat, and repeats to add the concentrated hydrochloric acid of 3ml mass fraction 36~38%, directly
It is generated to no Brown gas；
(4) it dissolves complex acid: adding the hydrochloric acid souring soln of 2ml mass fraction 0.36~0.38% into conical flask, then use wash bottle
To elute in a manner of inner wall solid-state precipitate, 7~8ml of distilled water is added, obtains complexing aqueous acid；
(5) oxydrolysis: the sodium hydroxide solution of mass fraction 20% is slowly added dropwise to molten in heating complexing aqueous acid to nearly boiling
Liquid has precipitating to generate, and the bromic acid sodium solution of 3ml mass fraction 10% is then added dropwise, and continues heating and keeps the slightly boiled 5min of solution, so
Sodium hydroxide solution and the 2ml mass fraction of 1ml mass fraction 10% is added dropwise respectively afterwards to continue to add for 10% bromic acid sodium solution
Heat makes solution slightly boiled 5 minutes, and adjusts pH value of solution to 8 ± 5, and the bromic acid sodium solution that addition 2ml mass fraction is 10% again is simultaneously
Continue to heat slightly boiled solution 5min, finally by the quick water cooling of solution to 15 DEG C hereinafter, static suspension 5min；
(6) rough segmentation platinum palladium component: taking sand core funnel and closely sealed with bottle,suction, connects suction filter pump, the solution in step (5) is poured into
Sand core funnel is opened suction filter pump and is filtered, purged conical flask inner wall 3 times with wash bottle, and cleaning solution is all moved to sand core funnel pumping
Filter, when in funnel precipitating filtered to it is close dry when, with wash bottle purging inner wall of hopper 3~4 times, make the precipitating for being adsorbed in inner wall of hopper
It is all collected on funnel sand core filter plate, finally drains precipitating, obtain high concentration cl sodium platinate filtrate；
(7) dissolution palladium precipitates hydrate: separately a bottle,suction is taken, by there are the sand core funnel of precipitating and bottle,suctions in step (6)
It is closely sealed, suction filter pump is connected, the concentrated hydrochloric acid of 1ml mass fraction 36~38% is added in sand core funnel, keeps precipitating in funnel whole
Dissolution purges inner wall of hopper with wash bottle, and by the precipitating for being adsorbed in inner wall, all purging is dissolved into acid solution in funnel, and suction filtration is used in combination
Wash bottle purges inner wall of hopper 3 times, makes in funnel not residual palladium solution, obtains maroon solution；
(8) it reoxidizes hydrolysis: resulting maroon solution being checked the number and is all moved into former conical flask, be placed on gas furnace and add
The bromic acid sodium solution of 4~5ml mass fraction 10% is added in heat, and when bubble-free in solution generates, mass fraction 5% is added dropwise
Sodium bicarbonate solution adjusts pH value of solution to 8 ± 5, palladium is made to be completely converted into dark brown precipitating and static solution 5min；
(9) second of separating platinum palladium component: a bottle,suction separately is taken, sand core funnel is closely sealed therewith, and suction filter pump in connection will walk
Suddenly the solution in (8) pours into sand core funnel, opens suction filter pump and filters, is purged conical flask inner wall 3 times with wash bottle, and cleaning solution is complete
Portion moves to sand core funnel suction filtration, when in funnel precipitating filtered to it is close dry when, with wash bottle purging inner wall of hopper 3~4 times, make to adsorb
It is all collected on funnel sand core filter plate in the precipitating of inner wall of hopper, finally drains precipitating, obtain low-level chlorinated sodium platinate filtrate；
(10) degradation sodium bromate: low-level chlorinated sodium platinate filtrate, which is moved in conical flask, to be placed in heat on natural gas furnace keeps its micro-
Boiling is added the concentrated hydrochloric acid of 3~4ml mass fraction 36~38%, is heated to solution and is concentrated by evaporation to 5ml, and step is added in three times
Suddenly the high concentration cl sodium platinate filtrate in (6), often plus a high concentration cl sodium platinate filtrate, add 3~4ml mass fraction 36~
38% concentrated hydrochloric acid is simultaneously close dry by solution heating, until solution heating is close dry；
(11) it generates ammonium chloroplatinate precipitate: the concentrated hydrochloric acid of 2ml mass fraction 36~38% being added into the conical flask of step (10)
Making to precipitate whole dissolutions with 10ml distilled water, then solution is fully transferred in beaker, heating beaker makes solution be warming up to 80 DEG C,
Agitating solution and point 4~5 addition 20g solid ammonium chlorides keep the temperature 5min after generating yellow ammonium chloroplatinate precipitate, and solution is quick
Water cooling stands 10min after cooling to room temperature；
(12) diafiltration ammonium chloroplatinate precipitate: sand core crucible is placed in a beaker, and carefully pours into potassium bichromate concentrated sulfuric acid solution to leaching
No crucible, take out sand core crucible after impregnating 30min, washes away washing lotion with tap water, distilled water will after eluting the inside and outside wall of sand core crucible
Sand core crucible is placed on bottle,suction, connects suction filter pump, distilled water is added in sand core crucible, cleans crucible sand with the mode of suction filtration
Core, clean sand core crucible are put into baking oven, under the conditions of 80 DEG C after constant temperature drying 1h, take out and are immediately placed in drier, cold
But to room temperature, sand core crucible net weight after cooling is weighed with assay balance, records weight W1；Sand core crucible is close with bottle,suction
It closes, yellow ammonium chloroplatinate precipitate in conical flask is fully transferred in sand core crucible, is adsorbed in conical flask by suction filter pump in connection
The ammonium chloroplatinate precipitate of wall all washes sand core crucible with saturated ammonium chloride solution, filters, and collects colorless filtrate；
(13) under suction filtration state, the ammonium chloride of ammonium chloroplatinate precipitate absorption diafiltration ammonium chloroplatinate precipitate: is washed away with dehydrated alcohol
Saturated solution；
(14) dry ammonium chloroplatinate precipitate: by there are the sand core crucibles of ammonium chloroplatinate precipitate to be put into beaker, cap upper surface ware is put
Entering to dry case, under the conditions of 90 DEG C, constant temperature drying 60min quickly removes beaker, puts into drier and be cooled to after completing drying
Room temperature；
(15) it calculates ammonium chloroplatinate precipitate quality: weighing ammonium chloroplatinate precipitate and sand core crucible gross mass W with assay balance2, then
Subtract sand core crucible net weight W1To get ammonium chloroplatinate mass M, according to formula: platinum content percentage value Pt%=(w in sample2-w1)
Platinum content percentage value in sample can be calculated in × 195/444 m × 100 ÷, in: W1For sand core crucible net weight, W2For chloroplatinic acid
Ammonia-sinking shallow lake and sand core crucible gross mass, m are sample quality, i.e. 0.3g.
2. platinum content measuring method in a kind of platinum-nickel alloys ornaments according to claim 1, which is characterized in that step (1)
In, sheet thickness 0.2mm.
3. platinum content measuring method in a kind of platinum-nickel alloys ornaments according to claim 1 or 2, which is characterized in that step
(1) in, platinum-nickel alloys sample blocks area < 1mm2。
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