CN109612795A - Impurities analysis detection method in a kind of tin and tin alloy - Google Patents
Impurities analysis detection method in a kind of tin and tin alloy Download PDFInfo
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- CN109612795A CN109612795A CN201811515551.6A CN201811515551A CN109612795A CN 109612795 A CN109612795 A CN 109612795A CN 201811515551 A CN201811515551 A CN 201811515551A CN 109612795 A CN109612795 A CN 109612795A
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Abstract
Impurities analysis detection method in a kind of tin and tin alloy, hydrochloric acid, the mixed solution of nitric acid or the mixed solution of hydrochloric acid, hydrogen peroxide is added in tin or tin alloy sample, heat resolve, and ensure that tin complete oxidation is tetravalent tin, then hydrochloric acid and heating evaporation is added to dry, repeat to be added hydrochloric acid and heating evaporation to dry step at least 3 times, this volatilization is complete until tinbase；Hydrochloric acid is added, continues to dissolve by heating completely, after cooling, is moved into volumetric flask, mixed, constant volume with water；Using the impurity element in any one measurement solution in spectrophotometer, Atomic Absorption Spectrometer, Atomic Fluorescence Spectrometer, inductively coupled plasma atomic emission spectrometer, icp ms, analysis detection obtains the impurity element in tin and tin alloy.Operation of the present invention is simple, environmental-friendly, high sensitivity, accuracy are good.
Description
Technical field
The invention belongs to metal detection analysis method technical fields, and in particular to the analysis of impurity element in tin and tin alloy
Detection method.
Background technique
The measurement of impurity element in tin and tin alloy, at present mainly using spectrophotometry, flame atomic absorption spectrometry,
Inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry.In order to reach impurity enriched and accurate
The purpose of measurement generallys use the interference that following several method eliminates tin:
1) hydrochloric acid-hydrobromic acid volatilization row's tin method." GB/T 3260-2013 tin chemical analysis method " mostly uses this method.It should
Method is most classic row's tin method, and advantage is that row's tin effect is good, easy to operate quick.The disadvantage is that hydrobromic acid has certain poison
Property, the simple substance bromine especially generated in reaction process are more toxic, handle additionally by which, and the elements such as arsenic, antimony can volatilize
Loss.
2) hydrogen chloride-chlorine volatilization row's tin method." YS/T 36-2011 high purity tin chemical analysis method " magnesium, aluminium, calcium, iron,
Cobalt, nickel, copper, zinc, silver, indium, gold, lead, Determine trace Bismuth use this method.This method advantage is that row's tin effect is good, and blank is low.Disadvantage
It is apparatus structure complexity, it is cumbersome, it is not easy to promote, the chlorine toxicity used is big, while the elements such as arsenic, antimony can volatilization loss.
3) extraction separation method.The measurement of " YS/T 36-2011 high purity tin chemical analysis method " antimony, using benzene extraction and separation
After measure antimony.This method it is maximum the disadvantage is that, cumbersome, the organic reagent toxicity used is big, and it is same to can not achieve multielement
When be enriched with.
4) Matrix phase or internal standard method.In " YS/T 746.17-2018 lead-free tin solder chemical analysis method " uses
Mark method is measured.The advantages of this method is simple and quick.The disadvantage is that impurity element not by enrichment, method Determination Limit compared with
It is high.Simultaneously when using inductively coupled plasma atomic emission spectrometry measurement, a large amount of tin matrix is easy with stannic oxide
Form be adsorbed in torch pipe, influence the service life of torch pipe.
Summary of the invention
For defect existing for existing tin and the various analyzing detecting methods of tin alloy, the object of the present invention is to provide one kind
It is simple to operate and friendly to environment, impurities analysis detection method in the tin and tin alloy that high sensitivity, accuracy are good.
The purpose of the present invention is achieved through the following technical solutions:
Impurities analysis detection method in a kind of tin and tin alloy, method and step are as follows:
(1) weigh tin or tin alloy sample, be added hydrochloric acid, nitric acid mixed solution or hydrochloric acid, hydrogen peroxide mixing
Solution in 80~200 DEG C of heat resolves, and ensures that tin complete oxidation is tin (IV), hydrochloric acid and heating evaporation is then added to dry,
Repeat to be added hydrochloric acid and heating evaporation to dry step at least 3 times, this volatilization is complete until tinbase；
(2) hydrochloric acid is added in the sample that will volatilize tin, continues to dissolve by heating completely, after cooling, be moved into volumetric flask with water,
It mixes, constant volume；
(3) spectrophotometer, Atomic Absorption Spectrometer, Atomic Fluorescence Spectrometer, inductively coupled plasma body atom are used
Any one measurement tin in emission spectrometer, icp ms or the impurity element in tin alloy.
Tin or tin alloy impurity element of the present invention include but is not limited to Ag, Al, As, Au, Bi, Ca, Cd, Ce, Co,
Cr、Cu、Fe、Ga、In、Mg、Ni、Pb、Sb、Zn。
Compared with the prior art, the present invention at least has the advantages that
1) operation of the present invention is easy, and the amount of reagent used is few, environmental-friendly.And the reagent used is easily purified, therefore is also fitted
Analysis for high purity tin product.
2) the remaining rate of tin is low, can remove 98% or more tin, and impurity residual is in the solution, preferably eliminates instrument
Matrix effects and other chemistry disruptions in continuous mode, improve Instrument measuring sensitivity.
3) after processed by the invention, require all impurity elements of measurement without significantly sacrificing (packet in tin and tin alloy product
Include the Volatile Elements such as As, Sb, Bi, Cr).
4) present invention cooperation inductively coupled plasma atomic emission spectrometry or inductively coupled plasma mass spectrometry make
With can reach the purpose of all impurity elements in tin and tin alloy product while measurement.
The method of the present invention is suitable for the tin such as high purity tin, tin slab, thick tin, tin-lead solder, lead-free solder and tin alloy product
The measurement of impurity element.
Specific embodiment
Embodiment 1
Impurities analysis detection method in tin and tin alloy, weigh 5.0g (being accurate to 0.0001g) high purity tin sample in
In 200mL quartz beaker, 15mL hydrochloric acid (1+1), 5mL nitric acid is added, is decomposed completely in 100 DEG C on temperature control electric furnace, keeps tin complete
It is oxidized to tetravalent tin i.e. tin (IV), and is evaporated to dryness, 2mL hydrochloric acid (1+1) then is added, is steamed in 100 DEG C of heating on temperature control electric furnace
It is sent to dry；It repeats that hydrochloric acid is added and heating evaporation is to dry step 5~6 time, this volatilization is complete until tinbase, tin matrix remnants rate
Down to less than 2%.2mL hydrochloric acid (1+1), 5mL water are added later, dissolves by heating sample, removes cooling, 10mL is moved into water and is held
In measuring bottle, mix.Using spectrophotometer, Atomic Absorption Spectrometer, Atomic Fluorescence Spectrometer, inductively coupled plasma body atom
Any one Instrument measuring tin in emission spectrometer, icp ms and the impurity element in tin alloy,
Including but not limited to Ag, Al, As, Au, Bi, Ca, Cd, Ce, Co,
Cr、Cu、Fe、Ga、In、Mg、Ni、Pb、Sb、Zn。
Embodiment 2
2.0g (being accurate to 0.0001g) refined tin sample is weighed in 200mL quartz beaker, addition 10mL hydrochloric acid (1+1),
3mL nitric acid decomposes completely in 120 DEG C on temperature control electric furnace, makes tin complete oxidation tetravalent tin, and be evaporated to dryness；2mL hydrochloric acid is added
(1+1) repeats this step (hydrochloric acid is added and heating evaporation to dry step) 4 in 120 DEG C of heating evaporations on temperature control electric furnace to dry
~5 times, until tinbase, this volatilization is complete.5mL hydrochloric acid (1+1), 5mL water are added later, in dissolving by heating sample on temperature control electric furnace,
Cooling is removed, is moved into 25mL volumetric flask with water, is mixed, using spectrophotometer, Atomic Absorption Spectrometer, atomic fluorescence light
Spectrometer, inductively coupled plasma atomic emission spectrometer, any one instrument in icp ms are surveyed
Determine the impurity element in tin and tin alloy, including but not limited to Ag, Al, As, Au, Bi, Ca, Cd, Ce, Co, Cr, Cu, Fe, Ga,
In、Mg、Ni、Pb、Sb、Zn。
Embodiment 3
1.0g (being accurate to 0.0001g) SnAg0.3Cu0.5 alloy is weighed in 200mL quartz beaker, 10mL hydrochloric acid is added
(1+1), 3mL nitric acid decomposes completely in 150 DEG C on temperature control electric furnace, makes tin complete oxidation tetravalent tin, and be evaporated to dryness；It is added
2mL hydrochloric acid (1+1), in 80 DEG C of heating evaporations on temperature control electric furnace to dry；This step 4~5 time are repeated, until tinbase is originally evaporated completely
Entirely；5mL hydrochloric acid (1+1), 5mL water is added and removes cooling in dissolving by heating sample on temperature control electric furnace, 25mL is moved into water and is held
In measuring bottle, mix, using spectrophotometer, Atomic Absorption Spectrometer, Atomic Fluorescence Spectrometer, inductively coupled plasma body atom
Any one Instrument measuring tin in emission spectrometer, icp ms and the impurity element in tin alloy,
Including but not limited to Ag, Al, As, Au, Bi, Ca, Cd, Ce, Co, Cr, Cu, Fe, Ga, In, Mg, Ni, Pb, Sb, Zn.
Embodiment 4
1.0g (being accurate to 0.0001g) SnCu0.7 alloy is weighed in 200mL quartz beaker, 10mL hydrochloric acid (1+ is added
1) sample is decomposed completely in 100 DEG C on temperature control electric furnace, makes tin complete oxidation tetravalent tin, and steam by, 2mL hydrogenperoxide steam generator
It is sent to dry；It is added 2mL hydrochloric acid (1+1), in 80 DEG C of heating evaporations on temperature control electric furnace to dry, repetition this step 3~4 time, Zhi Daoxi
Basic volatilization is complete；5mL hydrochloric acid (1+1), 5mL water is added, dissolves by heating sample, removes cooling, 25mL capacity is moved into water
It in bottle, mixes, is sent out using spectrophotometer, Atomic Absorption Spectrometer, Atomic Fluorescence Spectrometer, inductively coupled plasma body atom
Penetrate spectrometer, the impurity element in any one Instrument measuring tin and tin alloy in icp ms, packet
It includes but is not limited to Ag, Al, As, Au, Bi, Ca, Cd, Ce, Co, Cr, Cu, Fe, Ga, In, Mg, Ni, Pb, Sb, Zn.
Embodiment 5
The thick tin sample of 0.5g (being accurate to 0.0001g) is weighed in 200mL beaker, 6mL hydrochloric acid (1+1), 2mL nitric acid, in
It is decomposed completely for 200 DEG C on temperature control electric furnace, makes tin complete oxidation tetravalent tin, and be evaporated to dryness,；It is added 2mL hydrochloric acid (1+1), in
200 DEG C of heating evaporations repeat this step 3~4 time to doing on temperature control electric furnace, and until tinbase, this volatilization is complete；10mL hydrochloric acid is added,
10mL water is removed cooling, is moved into 100mL volumetric flask with water in dissolving by heating sample on temperature control electric furnace, mixes, using fire
The impurity elements such as flame aas determination Cu, Pb, Zn.
Claims (2)
1. impurities analysis detection method in a kind of tin and tin alloy, which is characterized in that steps are as follows:
(1) tin or tin alloy sample are weighed, hydrochloric acid, the mixed solution of nitric acid or the mixed solution of hydrochloric acid, hydrogen peroxide is added,
In 80~200 DEG C of heat resolves, and ensure that tin complete oxidation is tetravalent tin, hydrochloric acid then is added and heating evaporation is to doing, repeats
Hydrochloric acid and heating evaporation is added to dry step at least 3 times, this volatilization is complete until tinbase；
(2) hydrochloric acid is added in the sample that will volatilize tin, continues to dissolve by heating completely, after cooling, is moved into volumetric flask, mixed with water
It is even, constant volume；
(3) spectrophotometer, Atomic Absorption Spectrometer, Atomic Fluorescence Spectrometer, inductively coupled plasma body atomic emissions are used
The impurity element in any one measurement solution in spectrometer, icp ms, analysis detection obtain tin
And the impurity element in tin alloy.
2. impurities analysis detection method in a kind of tin according to claim 1 and tin alloy, which is characterized in that described
Tin or tin alloy impurity element include but is not limited to Ag, Al, As, Au, Bi, Ca, Cd, Ce, Co, Cr, Cu, Fe, Ga, In, Mg,
Ni、Pb、Sb、Zn。
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