CN106770221A - Method for determining mercury content in acid-making wastewater enriched by wet method - Google Patents
Method for determining mercury content in acid-making wastewater enriched by wet method Download PDFInfo
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Abstract
The invention discloses a method for determining mercury content in acid-making wastewater enriched by a wet method. The method adopts a copper reagent titration method to measure the mercury content in the mercury slag, and adds a certain amount of organic solvent carbon tetrachloride in the measuring process, so that the color change of the generated yellow copper diethylaminothiocarbamate dissolved in the carbon tetrachloride can be conveniently utilized to judge the reaction endpoint. Meanwhile, ascorbic acid and tartaric acid solution are added in the determination process, so that the interference of Fe can be eliminated synergistically, the accuracy and reliability of the result are ensured, in addition, the determination method provided by the invention does not need a mercury burning device, and the experiment consumables are reduced.
Description
Technical field
The invention belongs to chemical analysis technology field, and in particular to mercury content in a kind of measure wet-process beneficiation Wastewater from Acid Preparation
Method.
Background technology
Mercuric sulphide in zinc concentrate in zinc abstraction concentrate roasting process will be reduced and flash to mercuryvapour and enter dioxy
Change in sulphur flue gas, very big influence is caused to follow-up whole acid making system, environment and sulfuric acid quality.Acid in sulphuric acid process
Mercury in property waste water is by wet-process beneficiation in precipitation slag.
The assay method of domestic mercury mainly has volumetric method, photometry, atomic absorption spectrography (AAS), atomic fluorescence spectrometry, cold
Atomic absorption spectrography (AAS) etc..Volumetric method has rhodanate volumetric method, KI volumetric method.Rhodanate method result stabilization, determines
Wide ranges, however it is necessary that special device and consumptive material.KI volumetric determination mercury, iodide ion in acid medium, with mercury
（Ⅱ）Generate the mercuric iodixde precipitation of slightly solubility.The interference measurements such as silver-colored and substantial amounts of lead, copper and iron, after separated, these yuan
Element can be removed, but mercuric iodixde precipitation is too many, influences the observation of terminal.
The content of the invention
The invention aims to solve technical problem present in prior art, there is provided one kind is easy to observe terminal face
Color change, measurement result accurately and reliably, in a kind of experiment few measure wet-process beneficiation Wastewater from Acid Preparation of consumptive material mercury content method.
In order to achieve the above object, the present invention uses following technical scheme：One kind determines mercury in wet-process beneficiation Wastewater from Acid Preparation
The method of content, mercury slag is formed by the mercury wet-process beneficiation in acid waste water in precipitation slag, and the method is comprised the following steps：
A, the preparation of DDTC standard liquid and demarcation：Weigh a certain amount of DDTC and prepare DDTC standard liquid, after preparation
DDTC standard liquid is demarcated using mercury standard solution, is done blank test in company with demarcation and is calculated DDTC standard liquid
To the actual titer T of mercury；
B, the analysis of sample mercury slag and measure：
A, mercury slag sample to be measured pretreatment：Weigh 0.2g mercury slag samples to be measured to be placed in 150mL beakers, soaked with water, add
15mL nitric acid, micro-boiling is heated to after adding a cover surface plate, while adding 5mL hydrochloric acid, keeps dissolving 20min, sample under slight boiling condition
Dissolve and rinse wall of cup with water after cooling down completely, constant volume is in 100mL volumetric flasks；
B, sample content analysis：Divide to take pretreated sample solution 20mL in 250mL triangular flasks and Jia 2 and drip FeCl3Solution,
0.2~0.3g ascorbic acid, 10mL tartaric acid solutions and 2 drop copper acetate solutions are added, hydrogen-oxygen is used as indicator with phenolphthalein
Change ammonium and be neutralized to yellow disappearance and excessive 2~3 drop, add 5mL carbon tetrachloride, carbon tetrachloride is titrated to DDTC standard liquid
Occurs stabilization yellow in layer；
C, analysis result：The content of mercury in sample is calculated by following equation：
Actual titer of T --- the DDTC standard liquid to mercury；
V1--- the volume of the DDTC standard titration solution of titration sample consumption；
V0--- the volume of the DDTC standard liquid that titration mercury blank solution is consumed；
V2--- the cumulative volume of sample constant volume；
V3--- sample point takes volume；
M --- weigh sample mass.
Further, the preparation of the step A DDTC standard liquids is comprised the following steps with demarcation：
A, preparation：A certain amount of DDTC is weighed, 200mL ammonia solvents are used, 2L is diluted with water to, one week mistake is stood after shaking up
Filter, filtrate is to be calibrated；
B, demarcation：It is the mercury standard solution of 2.00mg/mL to draw 10.00mL concentration, is placed in 250mL triangular flasks, adds 5mL inverse
Chloroazotic acid, 2 drop FeCl3Solution, then adds 0.2~0.3g ascorbic acid, 10mL tartaric acid solutions and 2 drop copper acetate solutions,
50mL is diluted with water to, being neutralized to yellow using ammonium hydroxide as indicator with phenolphthalein disappears and excessive 2~3 drop, adds 5mL
After carbon tetrachloride, titrated with DDTC standard liquid, blank test is done in company with demarcating, by titration consumption DDTC standard liquid
The concentration and volume of volume and drawn mercury standard solution, calculate actual titer T of the DDTC standard liquid to mercury；
C, DDTC standard liquid is calculated by following equation to the actual titer T of mercury：
The actual titer of T --- DDTC standard liquid；
V4--- during demarcation, the volume of the DDTC standard titration solution that titration mercury standard solution is consumed；
V0--- during demarcation, the volume of the DDTC standard titration solution that titration mercury blank solution is consumed；
The concentration of c --- mercury standard solution；
V5--- draw the volume of mercury standard solution.
Further, yellow mercury oxide is titrated to DDTC standard liquid during sample content analysis in the step B to disappear
When very slow, indication terminal closes on, be aggressively shaken it is lower it is slow be titrated to carbon tetrachloride layer in there is stabilization yellow as terminal.
Further, surface plate will be added a cover when mercury slag sample to be measured is pre-processed in the step B up to micro- in electric boiling plate
Boiling.
The present invention has the advantages that compared with the prior art：The present invention be by the mercury wet-process beneficiation in acid waste water in
The preparation of DDTC standard liquid is carried out after in precipitation slag and is demarcated, then carried out the analysis of sample mercury slag and determine.The present invention
The mercury content in mercury slag is measured using DDTC titration, a certain amount of organic solvent four is added in continuous mode
Chlorination carbon, the change of color judges reaction eventually when being easy to be dissolved in carbon tetrachloride using the yellow diethylin bamic acid copper of generation
Point.Meanwhile, ascorbic acid and tartaric acid solution are added in continuous mode, the interference for eliminating Fe can be cooperateed with, ensure the standard of result
It is really reliable, in addition, assay method of the invention does not need the firing device of mercury, reduce experiment consumptive material.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
A kind of method for determining mercury content in wet-process beneficiation Wastewater from Acid Preparation, by the mercury wet-process beneficiation in acid waste water in precipitation
Mercury slag is formed in slag, the method is comprised the following steps：
A, the preparation of DDTC standard liquid and demarcation：
A, preparation：Weigh the DDTC of 2.4g（Analysis is pure）, 200mL ammonia solvents are used, 2L is diluted with water to, stand one after shaking up
Week filtering, filtrate is to be calibrated.
B, demarcation：It is the mercury standard solution of 2.00mg/mL to draw 10.00mL concentration, is placed in 250mL triangular flasks, is added
5mL（1+1）Inverse chloroazotic acid, 2 drop FeCl3Solution, then adds 0.2~0.3g ascorbic acid, 10mL tartaric acid solutions and 2 drop second
Sour copper solution, is diluted with water to 50mL, and yellow disappearance and excessive 2~3 are neutralized to using ammonium hydroxide as indicator with phenolphthalein
Drop, after adding 5mL carbon tetrachloride, is titrated with DDTC standard liquid, and blank test is done in company with demarcating, by titration consumption DDTC
The concentration and volume of the volume of standard liquid and drawn mercury standard solution, calculate actual drop of the DDTC standard liquid to mercury
Surely T is spent.
C, the numerical value in above-mentioned steps is brought into following equation calculate DDTC standard liquid to the actual titer T of mercury：
The actual titer of T --- DDTC standard liquid, unit（mg/mL）；
V4--- during demarcation, the volume of the DDTC standard titration solution that titration mercury standard solution is consumed, unit（mL）；
V0--- during demarcation, the volume of the DDTC standard titration solution that titration mercury blank solution is consumed, unit（mL）；
The concentration of c --- mercury standard solution, unit（mg/mL）；
V5--- draw the volume of mercury standard solution, unit（mL）.
Three parallel tests are carried out, it is actual titer of the DDTC standard liquid to mercury, result of calculation to choose average value
As shown in table 1.
Table 1:Result of calculation of the DDTC standard liquid to the actual titer of mercury
B, the analysis of sample mercury slag and measure：
A, mercury slag sample to be measured pretreatment：Weigh 0.2g mercury slag samples to be measured to be placed in 150mL beakers, soaked with water, add
15mL nitric acid, adds a cover surface plate after electric boiling plate up to micro-boiling, while adding 5mL hydrochloric acid, keeps being dissolved under slight boiling condition
20min, sample dissolving simultaneously rinses wall of cup after cooling with water completely, and constant volume is in 100mL volumetric flasks.
B, sample content analysis：Divide to take pretreated sample solution 20mL in 250mL triangular flasks and Jia 2 and drip FeCl3
Solution, adds 0.2~0.3g ascorbic acid, 10mL tartaric acid solutions and 2 drop copper acetate solutions, is used as indicator with phenolphthalein
Ammonium hydroxide is neutralized to yellow and disappears and excessive 2~3 drop, adds 5mL carbon tetrachloride, and yellow is titrated to DDTC standard liquid
When precipitation disappears very slow, indication terminal closes on, be aggressively shaken it is lower it is slow be titrated to carbon tetrachloride layer in there is stabilization yellow i.e.
It is terminal.
C, analysis result：The content of mercury in sample is calculated by following equation：
T --- DDTC standard liquid is to the actual titer of mercury, unit（mg/mL）；
V1--- the volume of the DDTC standard titration solution of titration sample consumption, unit（mL）；
V0--- the volume of the DDTC standard liquid that titration mercury blank solution is consumed, unit（mL）；
V2--- the cumulative volume of sample constant volume, unit（mL）；
V3--- sample point takes volume, unit（mL）；
M --- weigh sample mass, unit（g）.
The cubage result as shown in table 2 of mercury in sample
Table 2:The cubage result of mercury in sample
As shown in Table 2, using DDTC titration measuring mercury slag sample method simply efficiently, accurately and reliably.
The interference test of coexistence elements：
Each element content is in mercury slag：Arsenic, iron, aluminium, by after mercury slag sample to be measured pretreatment, coexistence elements and mercury enter together
Solution.This be accomplished by analysis coexistence elements whether interference measurement, mercury standard solution during titration, addition coexist accordingly
Element carries out interference test, as a result shows, the coexistence elements of addition are not interfered with to the analysis result of mercury content.
At the conditions of the experiments described above, by each replication of mercury slag sample to 3 different contents 6 times, mercury content is obtained
Test result relative standard deviation（RSD）As shown in table 3.
Table 3：Different each replications of mercury slag sample obtain the test result relative standard deviation of mercury content for 6 times（RSD）With
And the measurement result of distinct methods compares
From table 3 it can be seen that Wastewater from Acid Preparation enrichment obtains the measurement result relative standard deviation of mercury in mercury slag（RSD）It is 0.062
~0.11%, fully meet the requirement of analysis method.
Mark-on reclaims are tested：
Each 0.2000g of 1# and 3# samples in table 3 is weighed, mark-on reclaims experiment is carried out, experimental result as shown in table 4, draws mercury
Recovery of standard addition is respectively 99.31~101.15% and 99.57~101.27%, illustrates that result of the test of the invention disclosure satisfy that point
The requirement of analysis method.
Table 4：Mark-on reclaims result of the test
Claims (4)
1. it is a kind of determine wet-process beneficiation Wastewater from Acid Preparation in mercury content method, by the mercury wet-process beneficiation in acid waste water in precipitation slag
Middle formation mercury slag, it is characterised in that the method is comprised the following steps：
A, the preparation of DDTC standard liquid and demarcation：Weigh a certain amount of DDTC and prepare DDTC standard liquid, after preparation
DDTC standard liquid is demarcated using mercury standard solution, is done blank test in company with demarcation and is calculated DDTC standard liquid
To the actual titer T of mercury；
B, the analysis of sample mercury slag and measure：
A, mercury slag sample to be measured pretreatment：Weigh 0.2g mercury slag samples to be measured to be placed in 150mL beakers, soaked with water, add
15mL nitric acid, micro-boiling is heated to after adding a cover surface plate, while adding 5mL hydrochloric acid, keeps dissolving 20min, sample under slight boiling condition
Dissolve and rinse wall of cup with water after cooling down completely, constant volume is in 100mL volumetric flasks；
B, sample content analysis：Divide to take pretreated sample solution 20mL in 250mL triangular flasks and Jia 2 and drip FeCl3Solution,
0.2~0.3g ascorbic acid, 10mL tartaric acid solutions and 2 drop copper acetate solutions are added, hydrogen-oxygen is used as indicator with phenolphthalein
Change ammonium and be neutralized to yellow disappearance and excessive 2~3 drop, add 5mL carbon tetrachloride, carbon tetrachloride is titrated to DDTC standard liquid
Occurs stabilization yellow in layer；
C, analysis result：The content of mercury in sample is calculated by following equation：
Actual titer of T --- the DDTC standard liquid to mercury；
V1--- the volume of the DDTC standard titration solution of titration sample consumption；
V0--- the volume of the DDTC standard liquid that titration mercury blank solution is consumed；
V2--- the cumulative volume of sample constant volume；
V3--- sample point takes volume；
M --- weigh sample mass.
2. it is according to claim 1 it is a kind of determine wet-process beneficiation Wastewater from Acid Preparation in mercury content method, it is characterised in that：Institute
The preparation for stating step A DDTC standard liquids is comprised the following steps with demarcation：
A, preparation：A certain amount of DDTC is weighed, 200mL ammonia solvents are used, 2L is diluted with water to, one week mistake is stood after shaking up
Filter, filtrate is to be calibrated；
B, demarcation：It is the mercury standard solution of 2.00mg/mL to draw 10.00mL concentration, is placed in 250mL triangular flasks, adds 5mL inverse
Chloroazotic acid, 2 drop FeCl3Solution, then adds 0.2~0.3g ascorbic acid, 10mL tartaric acid solutions and 2 drop copper acetate solutions,
50mL is diluted with water to, being neutralized to yellow using ammonium hydroxide as indicator with phenolphthalein disappears and excessive 2~3 drop, adds 5mL
After carbon tetrachloride, titrated with DDTC standard liquid, blank test is done in company with demarcating, by titration consumption DDTC standard liquid
The concentration and volume of volume and drawn mercury standard solution, calculate actual titer T of the DDTC standard liquid to mercury；
C, DDTC standard liquid is calculated by following equation to the actual titer T of mercury：
The actual titer of T --- DDTC standard liquid；
V4--- during demarcation, the volume of the DDTC standard titration solution that titration mercury standard solution is consumed；
V0--- during demarcation, the volume of the DDTC standard titration solution that titration mercury blank solution is consumed；
The concentration of c --- mercury standard solution；
V5--- draw the volume of mercury standard solution.
3. it is according to claim 1 it is a kind of determine wet-process beneficiation Wastewater from Acid Preparation in mercury content method, it is characterised in that：Institute
When with DDTC standard liquid being titrated to yellow mercury oxide when stating sample content analysis in step B and disappearing very slow, indication terminal closes on,
Be aggressively shaken it is lower it is slow be titrated to carbon tetrachloride layer in there is stabilization yellow as terminal.
4. it is according to claim 1 it is a kind of determine wet-process beneficiation Wastewater from Acid Preparation in mercury content method, it is characterised in that：Institute
Stating when mercury slag sample to be measured is pre-processed in step B will add a cover surface plate in electric boiling plate up to micro-boiling.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459056A (en) * | 2017-08-18 | 2017-12-12 | 西北矿冶研究院 | Process for extracting mercury from acid-making wastewater by smelting flue gas |
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| CN101329277A (en) * | 2007-06-22 | 2008-12-24 | 上海市七宝中学 | Method for testing overproof of mercury contained in spot-removing cream |
| CN105092501A (en) * | 2015-09-23 | 2015-11-25 | 成都艾比科生物科技有限公司 | Method for determining mercury content in rapeseed oil |
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2016
- 2016-11-21 CN CN201611022608.XA patent/CN106770221A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329277A (en) * | 2007-06-22 | 2008-12-24 | 上海市七宝中学 | Method for testing overproof of mercury contained in spot-removing cream |
| CN105092501A (en) * | 2015-09-23 | 2015-11-25 | 成都艾比科生物科技有限公司 | Method for determining mercury content in rapeseed oil |
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| 童伟: "《食品检验、动植物检疫技术分析与管理实用大全》", 31 October 1999, 中国环境科学出版社 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107459056A (en) * | 2017-08-18 | 2017-12-12 | 西北矿冶研究院 | Process for extracting mercury from acid-making wastewater by smelting flue gas |
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