CN106706531A - Method for determining chloride ions in chromic anhydride by adopting silver chloride nephelometry - Google Patents
Method for determining chloride ions in chromic anhydride by adopting silver chloride nephelometry Download PDFInfo
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- CN106706531A CN106706531A CN201611243219.XA CN201611243219A CN106706531A CN 106706531 A CN106706531 A CN 106706531A CN 201611243219 A CN201611243219 A CN 201611243219A CN 106706531 A CN106706531 A CN 106706531A
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- chlorion
- chromic anhydride
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- G—PHYSICS
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- 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
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Abstract
The invention discloses a method for determining chloride ions in chromic anhydride by adopting silver chloride nephelometry. The method comprises the steps that a chromic anhydride sample is weighed and is dissolved with water in a beaker, and the chromic anhydride sample is transferred to a volumetric flask and diluted with water to reach a scale; two sample solution are taken in a brown volumetric flask, sulfuric acid, ferrous sulfate and ethylene glycol are added, and a silver nitrate solution is added to one solution; the solution is put in a dark place, the sample solution without silver nitrate is regarded as a reference solution, a turbidity value is measured at the wavelength of 440 nm by using an appropriate cuvette, and the amount of chloride ions is calculated from a working curve. The method can provide accurate data for chloride ion content in the chromic anhydride, fills the blank of determination of the chloride ion content in the chromic anhydride and is a simple, effective, rapid and practical method.
Description
Technical field
The present invention relates to a kind of starting material assay technology, specifically, it is related to chlorine in a kind of silver chlorate Nephelometric Determination chromic anhydride
The method of ion.
Background technology
Chromic anhydride is one of important source material of electroplating industry, and its quality good or not directly affects electroplating effect.If in plating
Chloride ion content is higher, it will coating is grown dim, covering power reduction, or even can make coating extra coarse and burnt hair.Therefore, it is necessary to tight
The content of chlorion in lattice control chromic anhydride.
But, lack in the prior art it is a kind of can quickly, in Accurate Determining chromic anhydride chloride ion content effective ways.
The content of the invention
Technical problem solved by the invention is to provide a kind of method of chlorion in silver chlorate Nephelometric Determination chromic anhydride, energy
Enough for the content of chlorion in chromic anhydride provides accurate data.
Technical scheme is as follows：
A kind of method of chlorion in silver chlorate Nephelometric Determination chromic anhydride, including：
Chromic anhydride sample is weighed, scale is diluted with water in beaker, immigration volumetric flask with water dissolves；
In taking two parts of sample solution brown volumetric flasks, plus sulfuric acid, ferrous sulfate, ethylene glycol, a copy of it adds silver nitrate molten
Liquid；
Dark place is placed, and is reference liquid to be not added with silver nitrate test solution, with suitable cuvette, turbidity is measured in wavelength 440nm
Value, obtains the amount of chlorion from working curve.
Further：
Sample 3.000g samples water dissolves are weighed in 300mL beakers, is moved into after dissolving in 250mL volumetric flasks, use water
Scale is diluted to, is mixed；
Two parts of 5.00mL solution are taken in 25mL brown volumetric flasks, plus 2mL concentration 1：1 sulfuric acid, 2.5mL concentration 100g/L
Ferrous sulfate, 10mL ethylene glycol；A copy of it adds 2mL concentration 10g/L silver nitrate solutiones, and scale is diluted to water, shakes up；
Under the protection of ethylene glycol, chlorion generates silver chlorate white precipitate with silver nitrate；30min is placed in dark place, with not
Plus silver nitrate test solution is reference liquid, with suitable cuvette, turbidity value is measured in wavelength 440nm, chlorine is obtained from working curve
The content of ion.
Further：In 25mL brown volumetric flasks, take respectively chlorion standard liquid 0,0.50,1.00,2.00,3.00,
4.00th, 5.00mL adds 2mL concentration 1：1 sulfuric acid, 10mL ethylene glycol, the silver nitrate solution of 2mL concentration 1% is diluted to quarter with water
Degree, shakes up；It is reference solution with not chloride ion-containing standard liquid, corresponding amount of chloride ions in solution is drawn with the turbidity value for measuring
Working curve.
Further：0.1648 gram of dry sodium chloride is weighed in 1000mL volumetric flasks, with water dissolves after, be diluted to quarter
Degree, shakes up, and the concentration of the chlorion standard liquid for obtaining is 0.1mg/mL.
Further：By formulaDraw the content of chlorion；
In formula, m1- Cl the amounts checked in from working curve, m- sample sizes, V- test solution cumulative volumes, V1- point take test solution volume.
Compared with prior art, the technology of the present invention effect includes：
The present invention can provide accurate data for the content of chlorion in chromic anhydride, fill up chlorion in measure chromic anhydride
The blank of content, method is simple, and operating personnel can grasp rapidly, be the content of chlorion in chromic anhydride, there is provided reliable number
According to.Therefore, it can extensive use, benefit has good prospects.
The present invention using chlorion in silver chlorate Nephelometric Determination chromic anhydride content, with it is quick, simple, be easy to grasp,
The features such as precision is good, the degree of accuracy is high.Suitable for upper measure of the chloride ion content between 0.04%-0.4% of production.
Specific embodiment
Technical solution of the present invention is elaborated below with reference to example embodiment.However, example embodiment can
Implement in a variety of forms, and be not understood as limited to implementation method set forth herein；Conversely, thesing embodiments are provided so that
The design of example embodiment more comprehensively and completely, and is comprehensively conveyed to those skilled in the art by the present invention.
The method of chlorion, specifically includes following steps in silver chlorate Nephelometric Determination chromic anhydride：
Step 1：Chromic anhydride sample is weighed, scale is diluted with water in beaker, immigration volumetric flask with water dissolves；
Sample 3.000g samples water dissolves are weighed in 300mL beakers, is moved into after dissolving in 250mL volumetric flasks, use water
Scale is diluted to, is mixed.
Step 2：In taking two parts of sample solution brown volumetric flasks, plus sulfuric acid, ferrous sulfate, ethylene glycol, a copy of it adds nitre
Sour silver solution；
Two parts of 5.00mL solution are taken in 25mL brown volumetric flasks, plus 2mL sulfuric acid (1+1), 2.5mL ferrous sulfate (100g/
L), 10mL ethylene glycol, a copy of it adds 2mL silver nitrate solutiones (10g/L), and another is not added with 2mL silver nitrate solutiones (10g/L),
Scale is diluted to water, is shaken up.
Step 3：Dark place is placed, and is reference liquid to be not added with silver nitrate test solution, with suitable cuvette, is surveyed in wavelength 440nm
Amount turbidity value, obtains the amount of chlorion from working curve.
Under the protection of ethylene glycol, chlorion generates silver chlorate white precipitate with silver nitrate, measures molten at 440nm wavelength
Liquid turbidity value.30min is placed in dark place, is reference liquid to be not added with silver nitrate test solution, with suitable cuvette, is surveyed in wavelength 440nm
Amount turbidity value, obtains the content of chlorion from working curve.
Step 31：The drafting of working curve；
Chromic anhydride：In 25mL brown volumetric flasks, chlorion standard liquid 0 is taken respectively, 0.50,1.00,2.00,3.00,
4.00,5.00mL (0.1mg/mL chlorion standard liquids：0.1648 gram of dry sodium chloride is weighed in 1000mL volumetric flasks,
After with water dissolves, scale is diluted to, shaken up) plus 2mL sulfuric acid (1+1), 10mL ethylene glycol, 2mL silver nitrate solutiones (1%), with water
Scale is diluted to, is shaken up, be reference solution with not chloride ion-containing standard liquid by aforesaid operations, with the turbidity value that measures to molten
Corresponding amount of chloride ions drawing curve in liquid.
Step 32：Draw the content of chlorion.
By formula：
In formula:m1- Cl amounts (mg) checked in from working curve, m- sample sizes (g), V- test solution cumulative volume (mL), V1- point
Take test solution volume, mL.
The tolerance of table 1
| Chlorinity (%) | Tolerance |
| <0.10 | 0.02 |
| 0.10~0.50 | 0.05 |
The chloride ion content of sample is 0.04~0.4% in actual production, because without standard sample thus carried out mark-on reclaims
Experiment, measurement result and the rate of recovery are shown in Table 2.
The chlorion recovery testu of table 2
| Sample ID | Chlorion standard value/% | Addition/% | Measured value/% | The rate of recovery/% |
| 1# | 0.030 | 0.040 | 0.068 | 97.1 |
Tested more than, select the consumption of optimum determining wavelength and suitable reducing agent and reducing agent, invented and adopted
With the content of chlorion in Nephelometric Determination chromic anhydride.
Term used herein is explanation and exemplary and nonrestrictive term.Because the present invention can be with various
Form specific implementation without deviating from invention it is spiritual or substantive, it should therefore be appreciated that above-described embodiment be not limited to it is any foregoing
Details, and widely being explained in the spirit and scope that should be limited in appended claims, thus fall into claim or its etc.
Whole changes and remodeling in the range of effect all should be appended claims and covered.
Claims (5)
1. in a kind of silver chlorate Nephelometric Determination chromic anhydride chlorion method, including：
Chromic anhydride sample is weighed, scale is diluted with water in beaker, immigration volumetric flask with water dissolves；
In taking two parts of sample solution brown volumetric flasks, plus sulfuric acid, ferrous sulfate, ethylene glycol, a copy of it adds silver nitrate solution；
Dark place is placed, and is reference liquid to be not added with silver nitrate test solution, with suitable cuvette, turbidity value is measured in wavelength 440nm, from
The amount of chlorion is obtained on working curve.
2. in silver chlorate Nephelometric Determination chromic anhydride as claimed in claim 1 chlorion method, it is characterised in that：
Sample 3.000g samples water dissolves are weighed in 300mL beakers, in moving into 250mL volumetric flasks after dissolving, dilute with water
To scale, mix；
Two parts of 5.00mL solution are taken in 25mL brown volumetric flasks, plus 2mL concentration 1：1 sulfuric acid, 2.5mL concentration 100g/L sulfuric acid
Ferrous iron, 10mL ethylene glycol；A copy of it adds 2mL concentration 10g/L silver nitrate solutiones, and scale is diluted to water, shakes up；
Under the protection of ethylene glycol, chlorion generates silver chlorate white precipitate with silver nitrate；30min is placed in dark place, to be not added with nitre
Sour silver test solution is reference liquid, with suitable cuvette, turbidity value is measured in wavelength 440nm, and chlorion is obtained from working curve
Content.
3. in silver chlorate Nephelometric Determination chromic anhydride as claimed in claim 2 chlorion method, it is characterised in that：In 25mL browns
In volumetric flask, chlorion standard liquid 0,0.50,1.00,2.00,3.00,4.00,5.00mL plus 2mL concentration 1 are taken respectively：1
Sulfuric acid, 10mL ethylene glycol, the silver nitrate solution of 2mL concentration 1% is diluted to scale with water, shakes up；It is molten with not chloride ion-containing standard
Liquid is reference solution, with the turbidity value that measures to corresponding amount of chloride ions drawing curve in solution.
4. in silver chlorate Nephelometric Determination chromic anhydride as claimed in claim 3 chlorion method, it is characterised in that：Weigh 0.1648
Gram dry sodium chloride in 1000mL volumetric flasks, with water dissolves after, be diluted to scale, shake up, the chlorion standard for obtaining is molten
The concentration of liquid is 0.1mg/mL.
5. in silver chlorate Nephelometric Determination chromic anhydride as claimed in claim 1 chlorion method, it is characterised in that：By formulaDraw the content of chlorion；In formula, m1- checked in from working curve
Cl amount, m- sample sizes, V- test solution cumulative volumes, V1- point take test solution volume.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611243219.XA CN106706531A (en) | 2016-12-29 | 2016-12-29 | Method for determining chloride ions in chromic anhydride by adopting silver chloride nephelometry |
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| CN201611243219.XA CN106706531A (en) | 2016-12-29 | 2016-12-29 | Method for determining chloride ions in chromic anhydride by adopting silver chloride nephelometry |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112304903A (en) * | 2020-10-16 | 2021-02-02 | 新疆众和股份有限公司 | Method for detecting concentration of chloride ions in turbid formed liquid |
| CN112557583A (en) * | 2020-12-22 | 2021-03-26 | 湖北省建筑科学研究设计院股份有限公司 | Method for detecting chloride ion content in concrete admixture by potentiometric titration |
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| JPH11311622A (en) * | 1998-04-30 | 1999-11-09 | Mitsubishi Materials Corp | Method and device for measuring halogen concentration by flow analysis method |
| CN102359944A (en) * | 2011-07-14 | 2012-02-22 | 内蒙古包钢钢联股份有限公司 | Determination method of chlorine content in iron-containing dust mud |
| CN104034683A (en) * | 2014-07-01 | 2014-09-10 | 大力电工襄阳股份有限公司 | Method for measuring chlorine content of vanadium battery electrolyte solution |
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2016
- 2016-12-29 CN CN201611243219.XA patent/CN106706531A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11311622A (en) * | 1998-04-30 | 1999-11-09 | Mitsubishi Materials Corp | Method and device for measuring halogen concentration by flow analysis method |
| CN102359944A (en) * | 2011-07-14 | 2012-02-22 | 内蒙古包钢钢联股份有限公司 | Determination method of chlorine content in iron-containing dust mud |
| CN104034683A (en) * | 2014-07-01 | 2014-09-10 | 大力电工襄阳股份有限公司 | Method for measuring chlorine content of vanadium battery electrolyte solution |
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| 安静等: "镀铬液中氯离子含量的测定", 《包钢科技》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112304903A (en) * | 2020-10-16 | 2021-02-02 | 新疆众和股份有限公司 | Method for detecting concentration of chloride ions in turbid formed liquid |
| CN112557583A (en) * | 2020-12-22 | 2021-03-26 | 湖北省建筑科学研究设计院股份有限公司 | Method for detecting chloride ion content in concrete admixture by potentiometric titration |
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Application publication date: 20170524 |
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