CN109633076A - The measuring method of Theil indices in the preprocess method and tin stripper of tin stripper - Google Patents
The measuring method of Theil indices in the preprocess method and tin stripper of tin stripper Download PDFInfo
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- CN109633076A CN109633076A CN201811502717.0A CN201811502717A CN109633076A CN 109633076 A CN109633076 A CN 109633076A CN 201811502717 A CN201811502717 A CN 201811502717A CN 109633076 A CN109633076 A CN 109633076A
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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
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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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
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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Abstract
This application involves the measuring methods of Theil indices in a kind of preprocess method of tin stripper and tin stripper.Wherein, the preprocess method of tin stripper is the following steps are included: provide tin stripper；The tin stripper and chloroazotic acid are mixed, heating resolution is obtained containing Sn4+Solution；Contain Sn for above-mentioned4+Solution and sulfuric acid solution mixing, be heated to sulfuric acid and smolder, the tin stripper that obtains that treated.The preprocess method of above-mentioned tin stripper, by the way that chloroazotic acid is added in tin stripper, heating resolution makes capacity of decomposition be strengthened, obtains containing Sn4+Solution, then by be added sulfuric acid solution, be heated to sulfuric acid and smolder, sample is further cleared up using concentrated sulfuric acid strong oxidizing property at high temperature and capacity of decomposition, while the nitric acid removed in sample of smoldering through persulfuric acid, the interference of nitric acid in subsequent measurements is eliminated, keeps measurement result more accurate and stablizes.
Description
Technical field
The present invention relates to technical field of analytical chemistry, more particularly in the preprocess method and tin stripper of a kind of tin stripper
The measuring method of Theil indices.
Background technique
Tin stripper, also known as stripping tin liquor, are one of primary chemical materials used in printed wiring board (PCB) production, use
In the stripping of tin coating, leypewter coating and soldered joint.Tin stripper can be divided into three types according to the difference of main component
Type:
(1) fluoride type tin stripper is made of hydrofluoric acid, villiaumite (ammonium acid fluoride), peroxide etc., since its environment refers to
Mark (fluoride high volatility, pollution are extremely heavy) and technical-economic index are poor, it has also become eliminate dosage form, use both at home and abroad now
It obtains less；
(2) nitric acid type tin stripper, by nitric acid, ferric nitrate, corrosion inhibiter, surfactant, nitrogen oxides inhibitor, complexing agent
Deng composition, concentration of nitric acid is generally 20%~25%, has high speed stripping tin, and high-efficient and lasting does not hurt bottom copper, and bright-copper-face is without greyish white
The features such as color；
(3) nitric acid-alkyl sulfonic acid type tin stripper, the composition of the dosage form is similar with nitric acid type tin stripper, and difference is only that nitre
Acid concentration is lower, general≤15%, reduce the harm to equipment and environment, but the addition of organic sulfonic acid mentions its cost slightly
It is high.Nitric acid type and nitric acid-alkyl sulfonic acid type tin stripper technical performance are close, are the leading dosage forms of current PCB production, 90% with
On especially medium-and-large-sized enterprise, PCB enterprise two kinds of tin strippers after use.
The analysis of Theil indices in tin stripper not only contributes to enterprise and improves production technology, optimization production procedure, and counterweight
The recycling and environmental protection of metal are of great significance.The measurement of Theil indices generally uses hydrochloric acid normal pressure in tin stripper at present
Resolution or micro-wave digestion, are completely dissolved tin in sample in the form of tin ion, add metal aluminium flake for the tetravalence in solution
Tin ion (Sn4+) it is reduced to divalent tin ion (Sn2+), divalent tin ion, which can be quantified, is reduced into iodide ion, Potassiumiodate for Potassiumiodate
Potassium and iodide ion reaction generate iodine, and iodine directing terminal blue in starch solution can be calculated by the Potassiumiodate consumed
Sample Theil indices.
However according to currently used tin stripper ingredient it is found that in tin stripper often containing a great deal of (generally 10%~
20%) nitric acid, and nitric acid has strong oxidizing property, the resolution of hydrochloric acid normal pressure or micro-wave digestion that presently relevant standard uses are difficult to
The nitric acid in sample to be tested is completely removed, remaining nitric acid generates dry when subsequent aluminium flake restores and Potassiumiodate titrates tin
It disturbs, makes unstable result, generate deviation.
Summary of the invention
Based on this, it is necessary to provide a kind of survey that can effectively improve Theil indices in the tin stripper for measuring Stability and veracity
Determine method.
In addition, the application also provides a kind of preprocess method of tin stripper.
A kind of preprocess method of tin stripper, comprising the following steps:
Tin stripper is provided；
The tin stripper and chloroazotic acid are mixed, heating resolution is obtained containing Sn4+Solution；
Described it will contain Sn4+Solution and sulfuric acid solution mixing, be heated to sulfuric acid and smolder, the tin stripper that obtains that treated.
Tin stripper is made of nitric acid, ferric nitrate, corrosion inhibiter, surfactant, nitrogen oxides inhibitor, complexing agent etc., at
Point more complicated, simple HCl treatment is often difficult to clear up completely, the preprocess method of the tin stripper of the application, by moving back tin
Chloroazotic acid is added in water, heating resolution makes capacity of decomposition be strengthened, obtains containing Sn4+Solution, then by be added sulfuric acid solution,
It is heated to sulfuric acid to smolder, further clears up sample using concentrated sulfuric acid strong oxidizing property at high temperature and capacity of decomposition, pass through simultaneously
Sulfuric acid is smoldered the nitric acid removed in sample, and the interference of nitric acid in subsequent measurements is eliminated, and is kept measurement result more accurate and is stablized.
The mass volume ratio of the tin stripper and chloroazotic acid is 1g:(20~50 in one of the embodiments) mL.
The temperature of the heating resolution is 100 DEG C~120 DEG C in one of the embodiments,.
The time of the heating resolution is 2min~3min in one of the embodiments,.
The mass volume ratio of the tin stripper and sulfuric acid solution is 1g:(10~25 in one of the embodiments) mL.
The volume ratio of the concentrated sulfuric acid and water is 1:1 in the sulfuric acid solution in one of the embodiments,.
The measuring method of Theil indices in a kind of tin stripper, comprising the following steps:
The tin stripper that the preprocess method of tin stripper described in any of the above embodiments is handled is provided；
In oxygen-free environment, obtained tin stripper and hydrochloric acid solution mixing are handled by described, metallic aluminium is added, is contained
Sn2+Solution；
Described it will contain Sn2+Solution use Potassiumiodate titration measuring, obtain the content of tin in tin stripper.
The volume ratio of concentrated hydrochloric acid and water is 1:1 in the hydrochloric acid solution in one of the embodiments,.
The mass ratio of the metallic aluminium and the tin stripper is 1:(0.1~0.25 in one of the embodiments).
The oxygen-free environment is maintained by the saturated sodium bicarbonate being added in reaction process in one of the embodiments,.
Specific embodiment
To facilitate the understanding of the present invention, below will to invention is more fully described, and give it is of the invention compared with
Good embodiment.But the invention can be realized in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
It should be noted that reagent used herein and water, when not indicating other and requiring refer both to analytical reagents and
Tertiary effluent specified in GB/T 6682--2008.Standard titration solution, preparation and product used in test are not indicating it
When he requires, prepared by the regulation of HG/T 3696.1, HG/T 3696.3.
The measuring method of Theil indices in the tin stripper of one embodiment, includes the following steps S110~S150:
S110, tin stripper is provided.
In the present embodiment, tin stripper by nitric acid, ferric nitrate, corrosion inhibiter, surfactant, nitrogen oxides inhibitor,
The composition such as complexing agent.
S120, above-mentioned tin stripper and chloroazotic acid are mixed, heating resolution is obtained containing Sn4+Solution.
Wherein, the mass volume ratio of tin stripper and chloroazotic acid is 1g:(20~50) ml.
Further, chloroazotic acid is the mixture that concentrated hydrochloric acid and concentrated nitric acid are 3:1 composition by volume.
It is appreciated that in the present embodiment, it is that 3:1 is first configured that chloroazotic acid, which can be concentrated hydrochloric acid and concentrated nitric acid by volume,
Mixed liquor, then be added tin stripper in；It is also possible to for concentrated hydrochloric acid and concentrated nitric acid being separately added into tin stripper, controls concentrated hydrochloric acid
Volume ratio with concentrated nitric acid is 3:1.
Further, the temperature for heating resolution is 100 DEG C~120 DEG C.The time of heating resolution is 2min~3min.
S130, contain Sn for above-mentioned4+Solution and sulfuric acid solution mixing, be heated to sulfuric acid and smolder, obtain that treated moves back tin
Water.
Wherein, the volume ratio of the concentrated sulfuric acid and water is 1:1 in sulfuric acid solution.
S140, in oxygen-free environment, treated tin stripper and hydrochloric acid solution are mixed, metallic aluminium is added, obtains
Containing Sn2+Solution.
Wherein, the volume ratio of concentrated hydrochloric acid and water is 1:1 in hydrochloric acid solution.
Further, the mass ratio of metallic aluminium and tin stripper is 1:(0.1~0.25).
By the way that metallic aluminium is added, the hydrogen generated using metallic aluminium and hydrochloric acid reaction is by Sn4+It is reduced into Sn2+。
Further, in the present embodiment, oxygen-free environment is the saturated sodium bicarbonate solution dimension being added in reaction process
It holds.Saturated sodium bicarbonate and hydrochloric acid reaction generate CO2, sucking air can be prevented, to prevent Sn2+By the oxygen oxygen in air
Change, and then influences the accuracy of measurement result.
Further, metal aluminium flake: mass fraction is not less than 99.5%, with a thickness of 0.1mm.
S150, contain Sn for above-mentioned2+Solution use Potassiumiodate titration measuring, obtain the content of tin in tin stripper.
It is appreciated that Sn2+It can quantify and Potassiumiodate is reduced into iodide ion, when titrating to terminal, Potassiumiodate and iodide ion
Reaction generates iodine, iodine directing terminal blue in starch solution.
Specifically, step S140~S150 are as follows: metal aluminium flake is added in testing liquid and blank solution, loads onto glass metal
Tube sealing stoppers rubber plug, and about 1/3 pipe saturated sodium bicarbonate solution is poured into pipe, is dissolved to aluminium flake, continues slightly boiled 3~5min.It is cold
But to room temperature, add saturated sodium bicarbonate solution at any time in the process (attention cannot allow it to suck air).By glass after cooling
Saturated sodium bicarbonate solution pours into conical flask in glass liquid sealing pipe, is rapidly added starch indicator solution, with Potassiumiodate titrand
Titration, being titrated to solution by the colourless blue that sports is terminal.
Wherein, Potassiumiodate standard titration solution: c (1/6KlO3)≈0.05mol/L.Starch indicator solution: 5g/L.
The content of tin based on mass fraction, is calculated as follows in tin stripper:
In formula:
V --- Potassiumiodate titrand volume consumed by burette test solution, unit are (ml)；
V0--- Potassiumiodate titrand volume consumed by titration blank solution, unit are (ml)；
C --- the concentration of Potassiumiodate standard solution, unit are mole every liter (mol/L)；
M --- sample quality, unit are gram (g)；
M --- tin (1/2Sn) molal weight, unit are gram every mole (g/mol) (M=59.35)
The measuring method of Theil indices, is cleared up using chloroazotic acid in above-mentioned tin stripper, and recycling sulfuric acid to smolder further makes
Sample decomposes, while removing nitric acid, eliminates the interference of nitric acid in subsequent measurements, keeps the result of measurement more accurate and stablizes,
Reproducibility significantly improves, and digestion time is short, easy to operate, greatly simplifies operating process, shortens analysis time.
The following are specific embodiments.
Embodiment 1
For the tin stripper for taking A factory to send as measuring samples, this sample appearance is in dark green, uses professional standard HG/ respectively
T4552.1-2013 and the present processes measure sample Theil indices, and sample is respectively measured in parallel 10 times.As a result as follows:
Table 1
As it can be seen from table 1 normal pressure resolution method Lower result and stability is poor, micro-wave digestion result is normal but due to not having
Have and thoroughly eliminate nitric acid interference, stability is also undesirable, and the measurement result of the application and stability are more satisfactory in contrast.By
Undesirable in normal pressure resolution method effect, comparison is all made of Microwave Digestion processing below.
Embodiment 2
The tin stripper for taking B factory and C factory to send respectively carries out Theil indices to sample as measuring samples, with the present processes
Measurement, sample are respectively measured in parallel 10 times, are measured Comparative result.As a result as follows:
Table 2
Embodiment 3
Continue to weigh tin stripper 0.3000g that B factory and C factory send as measuring samples, it is molten to be separately added into 10ml tin standard
Liquid (2mg/mL) carries out Sn assay with the present processes, repeats ten times, calculates average value, and Comparative result is as follows:
Table 3
Embodiment 4
The tin-stripping wastewater for taking D factory to send uses professional standard HG/T4552.1-2013 micro-wave digestion as measuring samples respectively
Facture and the method for the present invention measure Sn content, and sample is respectively measured in parallel 10 times, compares, see the table below to experimental condition:
Table 4
| Method | Analysis time/min | Equipment cost |
| HG/T4552.1-2013 | 100 | It is high |
| The application | 40 | It is lower |
The present processes are compared with industry standard methods HG/T4552.1-2013, by tin stripper pre-treating method
It improves, improves the Stability and veracity of measurement, be shown in Table 1~table 3, the application and industry standard methods HG/T4552.1-
2013, compared to analysis duration is shortened, improve efficiency, reduce analysis cost, be shown in Table 4.It is large quantities of that the application is particularly suitable for laboratory
Measure the measurement of tin-stripping wastewater Theil indices
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preprocess method of tin stripper, which comprises the following steps:
Tin stripper is provided；
The tin stripper and chloroazotic acid are mixed, heating resolution is obtained containing Sn4+Solution；
Described it will contain Sn4+Solution and sulfuric acid solution mixing, be heated to sulfuric acid and smolder, the tin stripper that obtains that treated.
2. the preprocess method of tin stripper according to claim 1, which is characterized in that the quality of the tin stripper and chloroazotic acid
Volume ratio is 1g:(20~50) mL.
3. the preprocess method of tin stripper according to claim 1, which is characterized in that it is described heating resolution temperature be
100 DEG C~120 DEG C.
4. the preprocess method of tin stripper according to claim 1 or 3, which is characterized in that the time of the heating resolution
For 2min~3min.
5. the preprocess method of tin stripper according to claim 1, which is characterized in that the tin stripper and sulfuric acid solution
Mass volume ratio is 1g:(10~25) mL.
6. the preprocess method of tin stripper according to claim 1 or 5, which is characterized in that dense sulphur in the sulfuric acid solution
The volume ratio of acid and water is 1:1.
7. the measuring method of Theil indices in a kind of tin stripper, which comprises the following steps:
The tin stripper that the preprocess method of the described in any item tin strippers of claim 1~6 is handled is provided；
In oxygen-free environment, obtained tin stripper and hydrochloric acid solution mixing are handled by described, metallic aluminium is added, obtains containing Sn2+'s
Solution；
Described it will contain Sn2+Solution use Potassiumiodate titration measuring, obtain the content of tin in tin stripper.
8. the measuring method of Theil indices in tin stripper according to claim 7, which is characterized in that dense in the hydrochloric acid solution
The volume ratio of hydrochloric acid and water is 1:1.
9. the measuring method of Theil indices in tin stripper according to claim 7, which is characterized in that the metallic aluminium with it is described
The mass ratio of tin stripper is 1:(0.1~0.25).
10. the measuring method of Theil indices in tin stripper according to claim 7, which is characterized in that the oxygen-free environment by
The saturated sodium bicarbonate being added in reaction process maintains.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113418917A (en) * | 2021-07-06 | 2021-09-21 | 广西博世科环保科技股份有限公司 | Analysis method for measuring aluminum content in aluminum ash by EDTA titration |
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