CN106404998B - The detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products - Google Patents
The detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products Download PDFInfo
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- CN106404998B CN106404998B CN201610920889.4A CN201610920889A CN106404998B CN 106404998 B CN106404998 B CN 106404998B CN 201610920889 A CN201610920889 A CN 201610920889A CN 106404998 B CN106404998 B CN 106404998B
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- G—PHYSICS
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- 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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Abstract
The present invention discloses a kind of detection method of Theil indices in high concentration of hydrogen tin oxide products.Described method includes following steps: sample to be tested is dissolved completely in concentrated hydrochloric acid by S1., forms stannic chloride solution to be measured；S2. under stiring, it is equivalent to 4 ~ 6 times of liquor capacity of dilute hydrochloric acid solution to be measured toward solution to be measured addition, obtains mixed liquor；S3. zinc powder is added several times into mixed liquor and carries out reduction reaction, S4. is added starch indicator into the clear and transparent solution of S3 gained, is titrated using Potassiumiodate standard solution, according to the Theil indices in titration results conversion stannic hydroxide；The mass content of tin element is not less than 30% in the sample to be tested.Detection method of the present invention, using the principle of reductometry, the reducing agent used by control and the addition manner for controlling reducing agent are still able to achieve stannic complete reduction for the sample of high tin content；Through repeatedly it is experimentally confirmed that testing result favorable reproducibility.
Description
Technical field
The invention belongs to chemical analysis fields, and in particular to the detection side of Theil indices in a kind of high concentration of hydrogen tin oxide products
Method.
Background technique
The detection method of common Theil indices, including atomic absorption spectrophotometry, inductively coupled plasma body emit light
Spectrometry, reductometry etc.；But the detection limit of these methods is normally no higher than 15%；Once the tin for measuring high-content produces
Product, testing result error is very big, poor reproducibility.
Contain a large amount of tin element in electrical type industrial wastewater, arbitrarily discharge can cause environmental pollution.Pass through precipitating
By its with stannic hydroxide recycling be a kind of waste utilization reasonable way, but this method obtain stannic hydroxide product in tin contain
It measures high, usually 30% or more, lacks a kind of content of tin in accurate detection stannic hydroxide product, to be difficult to this
The quality of product is managed.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide the inspections of Theil indices in high concentration of hydrogen tin oxide products
Survey method.The detection of the method Theil indices suitable for the sample of high tin concentration, favorable reproducibility.
Above-mentioned purpose of the invention is achieved by following technical solution:
The detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products, which comprises the steps of:
S1. sample to be tested is dissolved completely in concentrated hydrochloric acid, forms stannic chloride solution to be measured；
S2. under stiring, it is equivalent to 4~6 times of liquor capacity of dilute hydrochloric acid solution to be measured toward solution to be measured addition, is mixed
Close liquid；
S3. zinc powder is added several times into mixed liquor and carries out reduction reaction, and prevents air from entering reaction system；Add every time
1/2 of zinc powder quality needed for the zinc powder entered is not more than the whole sample to be tested stannic hydroxides of reduction；
The upper zinc powder being once added completely after completion of the reaction, then added next time；
Until mixed liquor, when being heated to 40~70 DEG C, solution is clear and transparent, stops the addition of zinc powder；
S4. starch indicator is added into the clear and transparent solution of S3 gained, is titrated using Potassiumiodate standard solution, root
According to the Theil indices in titration results conversion stannic hydroxide；
The mass content of tin element is not less than 30% in the sample to be tested.
When the prior art is using reductometry detection Theil indices, whether dissolved tetravalent tin is reduced into Bivalent Tin completely
It is the key factor for determining testing result accuracy, for the sample to be tested of low tin content, using existing method (such as aluminium
Piece reduction method) it is to be able to satisfy substantially, but for the sample of high tin content, acutely, reduction effect is poor, error for existing method reaction
Greatly.Inventors have found that being performed in multiple times reduction using zinc powder, the extent of reaction can be preferably controlled, it is ensured that for high tin content
Sample, be still able to achieve stannic complete reduction；Through repeatedly it is experimentally confirmed that testing result favorable reproducibility, provides one kind
Detect the detection method of Theil indices in high tin content sample.
The zinc powder is commercially available zinc powder, dark gray powder, Zn content > 99.9%.If selecting zinc metal sheet or size larger
Zinc granule, also it is more difficult maintain testing result reproducibility.Preferably, the partial size of the zinc powder is between 50~150 μm.
Preferably, in S1, sample to be tested is dissolved in the case where being heated to 80~100 DEG C.
Preferably, in S2, the mass concentration of the dilute hydrochloric acid is 15~20%.
From the angle being easier to operate to, it is preferable that in S3, the addition number of zinc powder is 2~4 times.More preferably 3 times.
In S3, the deal for the zinc powder being added every time can be identical or different, it is preferable that in S3, the zinc powder that is added every time
Quality is all the same.
Preferably, it in S3, is reacted to the addition of zinc powder next time completely from last zinc powder, is spaced 10~20 minutes.
Preferably, in S3, during zinc powder is added, by the way of fluid-tight, prevent air from entering system.
Preferably, in S4, the temperature of clear and transparent solution obtained by S3 is adjusted to room temperature, is rapidly added starch indicator,
It is titrated.
Preferably, the mass content of tin element is 30~60% in the sample to be tested.
Compared with prior art, the invention has the following beneficial effects:
Detection method of the present invention, using the principle of reductometry, the reducing agent used by control and control are also
The addition manner of former agent can still be able to achieve stannic complete reduction for the sample of high tin content；Card is tested repeatedly
Real, testing result favorable reproducibility provides a kind of detection method for detecting Theil indices in high tin content sample.
Specific embodiment
The present invention is made combined with specific embodiments below and further being elaborated, but embodiment is not the present invention
Any type of restriction.In embodiment, the percentage is calculated by mass percentage.Reagent used in embodiment, device
It is commercial device.
Stannic hydroxide sample to be measured in embodiment is the hydrogen-oxygen generated during recycling tin by tin stripper neutralization precipitation
Change tin solid.Theil indices are 30~60%.
Embodiment 1
S1. about 0.1g sample to be tested is dissolved completely in the 20mL concentrated hydrochloric acid that mass fraction is 37.5%, is heated to 90
DEG C, stirring is completely dissolved sample to be tested, is cooled to room temperature (25 DEG C), forms stannic chloride solution to be measured；
S2. solution to be measured obtained by S1 is placed on blender, control mixing speed is 100~200r/min, is added suitable
In 5 times of liquor capacity of dilute hydrochloric acid solution to be measured, mixed liquor is obtained；
S3. about 6g zinc powder (60 times of sample to be tested quality) are weighed, 3 parts is equally divided into, is added three times the mixed liquor of S2
In, the interval time that zinc powder is added every time is 10min, during zinc powder is added, with the glass that saturated sodium bicarbonate solution is housed
Glass liquid sealing pipe fluid-tight, prevents air from entering, until solution is heated to 60 DEG C, continues to stir after fully reacting, until solution is limpid
It is transparent.
S4. it is cooled to room temperature toward clear and transparent solution obtained by S3, is rapidly added 10mL starch indicator, uses Potassiumiodate mark
Quasi- solution rapid titration to solution becomes lazy, colour-fast in 30s, records Potassiumiodate consumption V, while doing blank test, records iodine
Sour potassium consumption V0, the Theil indices being calculate by the following formula out in stannic hydroxide.Sn (%)=(V-V0)×C×59.35/(10×
m)
Wherein C is the molar concentration of Potassiumiodate standard solution, and m is the quality of sample to be tested.
In specific embodiment, the concentration of Potassiumiodate standard solution is 0.0501mol/L.
Embodiment 2
The step of according to embodiment 1, difference is in S1, is heated to 80 DEG C.
Embodiment 3
The step of according to embodiment 1, difference is, in S3, weighs 6g zinc powder (60 times of sample to be tested quality), average mark
It is 2 parts, in the mixed liquor of point 2 addition S2.
Comparative example 1
The step of according to embodiment 1, difference is, in S3, using 6g aluminium flake be added at one time in the mixed solution of S2 into
Row reduction.
Comparative example 2
A sample is taken again, repeats the detection of comparative example 1.
Comparative example 3
The step of according to embodiment 1, difference is, in S3, using 6g zinc powder (60 times of sample to be tested quality)
It is added at one time in mixed liquor, is restored.
Comparative example 4
A sample is taken again, is repeated comparative example 3 and is detected.
Comparative example 5
The step of according to embodiment 1, difference is, in S3, using 6g zinc metal sheet (60 times of sample to be tested quality),
2 parts are equally divided into, in the mixed liquor of point 2 addition S2.
Comparative example 6
A sample is taken again, is repeated comparative example 5 and is detected.
The details of each embodiment and comparative example are as shown in table 1
Table 1
From Examples 1 to 3 as can be seen that using method of the present invention, the Theil indices of same sample to be tested are detected
As a result collimation is good.Especially suitable for the detection of high concentration Theil indices sample, from comparative example 1 and comparative example 2 and comparative example 3 with
Comparative example 4, comparative example 5 and comparative example 6, which can be seen that, uses existing method, or distribution is not used to add reducing agent, or
It is to replace zinc powder with zinc metal sheet, for the sample of high tin content, testing result poor reproducibility, therefore it is not suitable for high tin content
The measurement of sample.
Claims (8)
1. the detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products, which comprises the steps of:
S1. sample to be tested is dissolved completely in concentrated hydrochloric acid, forms stannic chloride solution to be measured；
S2. under stiring, it is added into solution to be measured and is equivalent to 4 ~ 6 times of liquor capacity of dilute hydrochloric acid solution to be measured, is mixed
Liquid；
S3. zinc powder is added several times into mixed liquor and carries out reduction reaction, and prevents air from entering reaction system；It is added every time
1/2 of zinc powder quality needed for zinc powder is not more than the whole sample to be tested stannic hydroxides of reduction；
The upper zinc powder being once added completely after completion of the reaction, then added next time；
Until mixed liquor, when being heated to 40 ~ 70 DEG C, solution is clear and transparent, stops the addition of zinc powder；
S4. starch indicator is added into the clear and transparent solution of S3 gained, is titrated using Potassiumiodate standard solution, according to drop
Determine the Theil indices in result conversion stannic hydroxide；
The mass content of tin element is not less than 30% in the sample to be tested.
2. according to claim 1 in high concentration of hydrogen tin oxide products Theil indices detection method, which is characterized in that in S1,
Sample to be tested is dissolved in the case where being heated to 80 ~ 100 DEG C.
3. according to claim 1 in high concentration of hydrogen tin oxide products Theil indices detection method, which is characterized in that in S2,
The mass concentration of the dilute hydrochloric acid is 15 ~ 20%.
4. according to claim 1 in high concentration of hydrogen tin oxide products Theil indices detection method, which is characterized in that in S3,
The addition number of zinc powder is 2 ~ 4 times.
5. the detection method of Theil indices according to claim 1 or in the 4 high concentration of hydrogen tin oxide products, which is characterized in that S3
In, the quality for the zinc powder being added every time is all the same.
6. according to claim 1 in high concentration of hydrogen tin oxide products Theil indices detection method, which is characterized in that in S3,
It is reacted to the addition of zinc powder next time completely from last zinc powder, is spaced 10 ~ 20 minutes.
7. according to claim 1 in high concentration of hydrogen tin oxide products Theil indices detection method, which is characterized in that in S3,
During zinc powder is added, by the way of fluid-tight, prevent air from entering system.
8. according to claim 1 in high concentration of hydrogen tin oxide products Theil indices detection method, which is characterized in that in S4,
The temperature of clear and transparent solution obtained by S3 is adjusted to room temperature, starch indicator is rapidly added, is titrated.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610920889.4A CN106404998B (en) | 2016-10-21 | 2016-10-21 | The detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products |
| PCT/CN2017/093294 WO2018072500A1 (en) | 2016-10-21 | 2017-07-18 | Method for detecting content of tin in high-concentration tin hydroxide product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610920889.4A CN106404998B (en) | 2016-10-21 | 2016-10-21 | The detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products |
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|---|---|
| CN106404998A CN106404998A (en) | 2017-02-15 |
| CN106404998B true CN106404998B (en) | 2019-01-22 |
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| WO (1) | WO2018072500A1 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404998B (en) * | 2016-10-21 | 2019-01-22 | 广州科城环保科技有限公司 | The detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products |
| CN108828134A (en) * | 2018-09-05 | 2018-11-16 | 苏州宝士杰塑料科技有限公司 | Stannous measurement solution and its application method |
| CN109633076A (en) * | 2018-12-10 | 2019-04-16 | 广东省佛山地质局(广东省佛山地质灾害应急抢险技术中心) | The measuring method of Theil indices in the preprocess method and tin stripper of tin stripper |
| CN114739781A (en) * | 2022-04-22 | 2022-07-12 | 浙江恒祥检测技术服务有限公司 | Novel wet digestion method |
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| CN104215634A (en) * | 2014-09-16 | 2014-12-17 | 湖南有色新田岭钨业有限公司 | Method for determining content of tin in tungsten concentrate |
| CN104515826A (en) * | 2014-11-29 | 2015-04-15 | 江西洪都航空工业集团有限责任公司 | Method for determination of tin content in tin-lead solder by complexometric titration method |
| CN105021545A (en) * | 2015-07-09 | 2015-11-04 | 江南工业集团有限公司 | Method for measuring contents of bismuth and lead ions in tin lead bismuth alloy electroplating solution |
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| US2716596A (en) * | 1952-01-18 | 1955-08-30 | Nat Steel Corp | Determination of tin on tinplate |
| CN102735793A (en) * | 2011-04-08 | 2012-10-17 | 新疆独山子天利实业总公司 | Improved determination method for improving content of melting tin in maleate tin oxide |
| CN105548460B (en) * | 2015-12-30 | 2018-01-26 | 东旭科技集团有限公司 | A kind of method for determining stannous oxide content |
| CN106404998B (en) * | 2016-10-21 | 2019-01-22 | 广州科城环保科技有限公司 | The detection method of Theil indices in a kind of high concentration of hydrogen tin oxide products |
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- 2016-10-21 CN CN201610920889.4A patent/CN106404998B/en not_active Expired - Fee Related
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104215634A (en) * | 2014-09-16 | 2014-12-17 | 湖南有色新田岭钨业有限公司 | Method for determining content of tin in tungsten concentrate |
| CN104515826A (en) * | 2014-11-29 | 2015-04-15 | 江西洪都航空工业集团有限责任公司 | Method for determination of tin content in tin-lead solder by complexometric titration method |
| CN105021545A (en) * | 2015-07-09 | 2015-11-04 | 江南工业集团有限公司 | Method for measuring contents of bismuth and lead ions in tin lead bismuth alloy electroplating solution |
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| CN106404998A (en) | 2017-02-15 |
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