CN106323890A - Method for measuring calcium and magnesium ions in pressure filtrate of zinc smelting and purifying process - Google Patents
Method for measuring calcium and magnesium ions in pressure filtrate of zinc smelting and purifying process Download PDFInfo
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- CN106323890A CN106323890A CN201610689617.8A CN201610689617A CN106323890A CN 106323890 A CN106323890 A CN 106323890A CN 201610689617 A CN201610689617 A CN 201610689617A CN 106323890 A CN106323890 A CN 106323890A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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Abstract
The invention relates to a method for measuring calcium and magnesium ions in pressure filtrate of a zinc smelting and purifying process. The method comprises the following steps: (1) adding an acid into the pressure filtrate of the zinc smelting and purifying process, regulating the acidity, and controlling the pH value to be 3-5; (2) adding 100-150g of soluble barium salt into the solution in the step (1) per liter, and standing for 10-15 minutes; (3) adding 20-50g of alums into the solution in the step (2) per liter after standing is ended, and standing for 10-15 minutes; (4) filtering the solution obtained in the step (3), and remaining the filtrate; and (5) measuring the concentration of the calcium and magnesium ions in the filtrate in the step (4) by flame atomic absorption spectrometry. According to the method, perchloric acid is added into the pressure filtrate of the zinc smelting and purifying process, so that sulfate ions in the solution can be completely released; due to the added soluble barium salt, the sulfate ions in the solution can be effectively removed, the measurement method is simple, convenient, high in efficiency and accurate in measurement, and the measurement cost can be effectively reduced.
Description
Technical field
The present invention relates to the assay method of a kind of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions.
Background technology
At present in zinc metallurgical process, owing to containing calcium, magnesium ion in solution, cleaning procedure carries out solution pressure-filtering process
In, the calcium ions and magnesium ions in solution is constantly enriched with and increases, when the calcium in solution, magnesium ion increase to finite concentration, and calcium, magnesium ion are just
Can be adsorbed in a large number on filter plate and filter cloth, be easily caused that filter cloth limit is hardening, filter plate liquid outlet is blocked by calcium and magnesium crystallization, impact pressure
The filter pressing performance of filter.Measure the calcium in pressing filtering liquid, magnesium ion content timely and accurately, the most do not surpass at calcium, magnesium ion content
Clear up absorption calcium and magnesium crystallization on filter plate and filter cloth when target in time, can avoid the occurrence of that filter cloth limit is hardening, filter plate liquid outlet
Blocked by calcium and magnesium crystallization, affect the situation of the filter pressing performance of pressure filter.At present can Accurate Determining zinc abstraction cleaning procedure pressing filtering liquid
The method of calcium ions and magnesium ions content, step is more and complex, adds the labor intensity of employee, adds production cost；And
The easy assay method measuring pressing filtering liquid calcium ions and magnesium ions content, measurement result is inaccurate, it is difficult to instruct commercial production.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide one and measure accurate, determination efficiency height and measure into
The assay method of this low zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions.
For achieving the above object, the present invention provides techniques below scheme:
The assay method of a kind of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that comprise the following steps:
(1) containing Ca2+100-500mg/L, Mg2+The zinc abstraction cleaning procedure pressing filtering liquid of 100-500mg/L adds acid, regulation
Acidity, controls pH=3-5；
(2) in every liter of step (1) solution, add the soluble barium salt of 100g-150g, stand 10-15min；
(3), after standing terminates, every liter of step (2) solution adds the Alumen of 20-50 gram, stands 10-15min；
(4) solution that step (3) obtains is filtered, leave filtrate；
(5) by the concentration of calcium ions and magnesium ions in the filtrate in Flame Atomic Absorption Spectrometry Determination step (4).
Preferably, the acid in described step (1) is perchloric acid.
Preferably, the soluble barium salt in described step (2) is any one in barium chloride, barium nitrate, barium hydroxide.
Preferably, the filtration in described step (4) refers to filtration under diminished pressure.
Preferably, described step (2) adds in every liter of step (1) solution the soluble barium salt of 125g.
Above-mentioned steps (1) adds in zinc abstraction cleaning procedure pressing filtering liquid perchloric acid, can be by zinc abstraction cleaning procedure
Pressing filtering liquid is adjusted to acidity, and perchloric acid has strong oxidizing property simultaneously, can make the sulfate radical in zinc abstraction cleaning procedure pressing filtering liquid
Discharge completely under the conditions of acidity, Strong oxdiative.
Adding soluble barium salt in above-mentioned steps (2), soluble barium salt can be with the sulfur that discharges completely in step (1)
Acid group reaction generates barium sulfate precipitate, effectively eliminates sulfate ion in zinc abstraction cleaning procedure pressing filtering liquid.
Above-mentioned steps (3) adds Alumen absorption barium sulfate precipitate, then carries out filtration treatment removing barium sulfate, sulphuric acid can be made
Precipitated barium removal effect is more preferable, and in effective elimination solution, barium sulfate precipitate is to calcium and magnesium in Flame Atomic Absorption Spectrometry Determination filtrate
The impact of the concentration of ion.
It is an advantage of the current invention that in zinc abstraction cleaning procedure pressing filtering liquid, first add perchloric acid, regulate acidity, control pH
=3-5, can discharge the sulfate ion in solution completely under the conditions of acidity, Strong oxdiative, add soluble barium salt, produces
Barium sulfate precipitate, can effectively remove the sulfate ion in solution, adds the barium sulfate in Alumen adsorption precipitation solution, can remove
Go in solution barium sulfate precipitate on the impact of the concentration of calcium ions and magnesium ions in Flame Atomic Absorption Spectrometry Determination filtrate.Than tradition
The assay method of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, assay method is easy, and determination efficiency is high and measurement result is accurate,
Can effectively instruct commercial production, reduce calcium ions and magnesium ions cost of determination simultaneously.
Detailed description of the invention
The following examples can help those skilled in the art that the present invention is more fully understood, but cannot be with any
Mode limits the present invention.
Embodiment 1
The assay method of a kind of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that comprise the following steps:
(1) 1L is taken containing Ca2+100mg/L, Mg2+The zinc abstraction cleaning procedure pressing filtering liquid of 100mg/L, adds perchloric acid, regulation acid
Degree, controls pH=3；
(2) in step (1) solution, add the barium chloride of 100g, stand 10min；
(3), after standing terminates, step (2) solution adds the Alumen of 20 grams, stands 10min；
(4) solution that step (3) obtains is carried out filtration under diminished pressure, leave filtrate；
(5) by the concentration of calcium ions and magnesium ions in the filtrate in Flame Atomic Absorption Spectrometry Determination step (4).
Embodiment 2
The assay method of a kind of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that comprise the following steps:
(1) 1L is taken containing Ca2+500mg/L, Mg2+The zinc abstraction cleaning procedure pressing filtering liquid of 500mg/L, adds perchloric acid, regulation acid
Degree, controls pH=5；
(2) in step (1) solution, add the barium nitrate of 150g, stand 15min；
(3), after standing terminates, step (2) solution adds the Alumen of 50 grams, stands 15min；
(4) solution that step (3) obtains is carried out filtration under diminished pressure, leave filtrate；
(5) by the concentration of calcium ions and magnesium ions in the filtrate in Flame Atomic Absorption Spectrometry Determination step (4).
Embodiment 3
The assay method of a kind of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that comprise the following steps:
(1) 1L is taken containing Ca2+300mg/L, Mg2+The zinc abstraction cleaning procedure pressing filtering liquid of 300mg/L, adds perchloric acid, regulation acid
Degree, controls pH=4；
(2) in step (1) solution, add the barium hydroxide of 125g, stand 12min；
(3), after standing terminates, step (2) solution adds the Alumen of 35 grams, stands 12min；
(4) solution that step (3) obtains is carried out filtration under diminished pressure, leave filtrate；
(5) by the concentration of calcium ions and magnesium ions in the filtrate in Flame Atomic Absorption Spectrometry Determination step (4).
Comparative example 1
Compared with Example 1, comparative example 1 does not carries out step (3) and processes, and remaining step is the most same as in Example 1.
The present invention chooses containing Ca2+300mg/L, Mg2+The zinc abstraction cleaning procedure pressing filtering liquid 120 parts of 300mg/L is right for research
As, every part of 1L.Being below the determination test of 6 groups of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, often group 20 parts, does having a competition
Test: wherein A, B, component C do not use the assay method of the zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions in embodiment 1-3 to survey
Fixed, the assay method that D group uses ethylenediaminetetraacetic acid to demarcate calcium ions and magnesium ions concentration measures, and E group is for using inductive coupling plasma
Body emission spectrometer assay, F group uses the mensuration side of the zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions in comparative example 1
Method measures, result such as table 1.
Table 1
| Packet | Calcium ion content | Magnesium ion content | Mensuration expense (first) | Measure time-consuming |
| A | 295.62mg/L | 298.76mg/L | 120 | 48min |
| B | 296.56mg/L | 297.63mg/L | 120 | 51min |
| C | 298.68mg/L | 296.52mg/L | 120 | 50min |
| D | 286.34mg/L | 285.72mg/L | 160 | 62min |
| E | 281.87mg/L | 273.91mg/L | 180 | 60min |
| F | 290.01mg/L | 289.98mg/L | 120 | 38min |
It is not difficult to find out the assay method than tradition zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, this mensuration side by the above results
The determination efficiency of method is high and measurement result is accurate, can effectively instruct commercial production, reduce calcium ions and magnesium ions cost of determination simultaneously.
Although, the present invention is described in detail the most with a general description of the specific embodiments, but
On the basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (5)
1. the assay method of a zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that comprise the following steps:
(1) containing Ca2+100-500mg/L, Mg2+The zinc abstraction cleaning procedure pressing filtering liquid of 100-500mg/L adds acid, regulation acid
Degree, controls pH=3-5；
(2) in every liter of step (1) solution, add the soluble barium salt of 100g-150g, stand 10-15min；
(3), after standing terminates, every liter of step (2) solution adds the Alumen of 20-50 gram, stands 10-15min；
(4) solution that step (3) obtains is filtered, leave filtrate；
(5) by the concentration of calcium ions and magnesium ions in the filtrate in Flame Atomic Absorption Spectrometry Determination step (4).
A kind of assay method of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that
Acid in step (1) is perchloric acid.
A kind of assay method of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that
Soluble barium salt in step (2) is any one in barium chloride, barium nitrate, barium hydroxide.
A kind of assay method of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that
Filtration in step (4) refers to filtration under diminished pressure.
A kind of assay method of zinc abstraction cleaning procedure pressing filtering liquid calcium ions and magnesium ions, it is characterised in that
Step (2) adds in every liter of step (1) solution the soluble barium salt of 125g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610689617.8A CN106323890A (en) | 2016-08-19 | 2016-08-19 | Method for measuring calcium and magnesium ions in pressure filtrate of zinc smelting and purifying process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610689617.8A CN106323890A (en) | 2016-08-19 | 2016-08-19 | Method for measuring calcium and magnesium ions in pressure filtrate of zinc smelting and purifying process |
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| CN106323890A true CN106323890A (en) | 2017-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610689617.8A Pending CN106323890A (en) | 2016-08-19 | 2016-08-19 | Method for measuring calcium and magnesium ions in pressure filtrate of zinc smelting and purifying process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106383089A (en) * | 2016-08-29 | 2017-02-08 | 南丹县南方有色金属有限责任公司 | Determination method of calcium and magnesium ions in press-filtrate of zinc smelting purification process |
| JP2021056201A (en) * | 2019-09-28 | 2021-04-08 | 杭州力松電子科技有限公司 | Facility to automatically measure concentration of sulfuric acid salt solution |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58740A (en) * | 1981-06-26 | 1983-01-05 | Toshiba Corp | Determination of trace element in gallium-arsenic |
| CN1699970A (en) * | 2005-07-01 | 2005-11-23 | 北京博晖创新光电技术股份有限公司 | Atom absorption method and apparatus for multi-element simultaneous determination |
| CN102507279A (en) * | 2011-10-14 | 2012-06-20 | 安徽皖仪科技股份有限公司 | Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid |
| CN105779793A (en) * | 2016-02-03 | 2016-07-20 | 河南永银化工实业有限公司 | Method for separating micro-uranium from bittern through coprecipitation method |
-
2016
- 2016-08-19 CN CN201610689617.8A patent/CN106323890A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58740A (en) * | 1981-06-26 | 1983-01-05 | Toshiba Corp | Determination of trace element in gallium-arsenic |
| CN1699970A (en) * | 2005-07-01 | 2005-11-23 | 北京博晖创新光电技术股份有限公司 | Atom absorption method and apparatus for multi-element simultaneous determination |
| CN102507279A (en) * | 2011-10-14 | 2012-06-20 | 安徽皖仪科技股份有限公司 | Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid |
| CN105779793A (en) * | 2016-02-03 | 2016-07-20 | 河南永银化工实业有限公司 | Method for separating micro-uranium from bittern through coprecipitation method |
Non-Patent Citations (2)
| Title |
|---|
| 俞娟 等: "锌的常压富氧直浸工艺及钙镁结晶特征研究", 《湿法冶金》 * |
| 李文波 等: "原子吸收光谱法测定硫酸盐型卤水中钙", 《光谱实验室》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106383089A (en) * | 2016-08-29 | 2017-02-08 | 南丹县南方有色金属有限责任公司 | Determination method of calcium and magnesium ions in press-filtrate of zinc smelting purification process |
| JP2021056201A (en) * | 2019-09-28 | 2021-04-08 | 杭州力松電子科技有限公司 | Facility to automatically measure concentration of sulfuric acid salt solution |
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Application publication date: 20170111 |