CN110231435A - A kind of method of chloride content determination in aluminium wastewater - Google Patents
A kind of method of chloride content determination in aluminium wastewater Download PDFInfo
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- CN110231435A CN110231435A CN201910681240.5A CN201910681240A CN110231435A CN 110231435 A CN110231435 A CN 110231435A CN 201910681240 A CN201910681240 A CN 201910681240A CN 110231435 A CN110231435 A CN 110231435A
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- ammonium thiocyanate
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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
- 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 relates to analysis technical fields.Influence of the aluminium ion to test result is avoided with the chloride ion in excessive silver nitrate solution deposit sample using Fo Erhadefa；It is titrated respectively under identical acidity environmental condition, the ammonium thiocyanate volume differences of consumption is converted into chlorine ion concentration.The method of chloride content determination in aluminium wastewater of the present invention, using Fo Erhadefa, prepare including 1) reagent and indicator, 2) preparation of samples, 3) titration and 4) calculating process, under identical strong acidic condition, blank and water sample to be measured are titrated respectively, the ammonium thiocyanate standard solution volume of consumption is denoted as V respectively0And V1；It presses
Description
Technical field
The present invention relates to analysis technical field, it is related to chlorinity in aluminium content measuring technology more particularly to aluminium wastewater and surveys
Determine technology.
Background technique
Document is gravimetric method, titration, chromatography of ions etc. to the measuring method of Chloride Ion In Water content at present, however
There is a large amount of aluminium ion in water, in the detection process to water sample or because indicator inactivates, or because analytical column is not resistant to aluminium
Ion is limited.Or the limitation based on method itself, can not Accurate Determining such Chloride Ion In Water content.
Conventional detection method is to titrate chloride ion with silver nitrate standard solution, and indicator is potassium chromate.But due to depositing
A large amount of chromic acid aluminum precipitation can be generated after indicator is added in a large amount of aluminium ion, be will lead to indicator in this way and lost work
Property, influence test accuracy.
In view of the above-mentioned problems, the present invention provides a kind of method of chloride content determination in aluminium wastewater, by adding in water
Enter excess nitric acid silver solution, so that chloride ion is completely converted into silver nitride precipitation, remaining silver ion is under conditions of pH is acid
Make indicator with ammonium ferric sulfate, in the presence of aluminium ion, with the silver ion of ammonium thiocyanate standard solution overtitration.Compared to direct
The method present invention does not have to processing aluminium ion and the relationship that reacts of potassium chromate indicator, avoid potassium chromate indicator inactivation because
Element, method are efficient and convenient.Accuracy rate is high, favorable reproducibility.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of chloride content determination in aluminium wastewater.
The principle of the present invention are as follows: for blank reference being done with distilled water, using Fo Erha containing a large amount of aluminum ions water samples
Moral method avoids influence of the aluminium ion to test result in waste water, with the excess nitric acid silver solution of equivalent precipitate respectively chlorinated water sample and
Chloride ion in distilled water reference；It is molten with ammonium thiocyanate standard with ammonium ferric sulfate indicator under the conditions of identical acidic environment
Liquid titrates processed sample containing aluminum and reference respectively, and the ammonium thiocyanate volume differences of two sample consumptions are converted into sample
Chlorine ion concentration in product.
The method of chloride content determination in aluminium wastewater of the present invention, using Fo Erhadefa, including 1) reagent and finger
Show agent preparation, 2) preparation of samples, 3) titration and 4) calculating process, it is characterised in that:
1) reagent and indicator prepare: the reagent includes silver nitrate solution, nitric acid solution and ammonium thiocyanate standard solution；Sulfuric acid
Iron ammonium indicator；
2) preparation of samples: using distilled water as blank；Water sample to be measured is filtered through middling speed quantitative filter paper；
3) titrate: including sample titration and blank titration, under identical strong acidic condition, respectively to blank and water sample to be measured into
Row titration, the ammonium thiocyanate standard solution volume of consumption are denoted as V respectively0And V1；
4) calculate: the chlorinity x of sample calculates as follows:
In formula: C --- ammonium thiocyanate concentration of standard solution, mol/l；
V0--- the ammonium thiocyanate volume of reference sample consumption, ml；
V1--- the ammonium thiocyanate volume of sample consumption, ml；
M --- sample to be tested quality, %wt.
The method of chloride content determination in aluminium wastewater of the present invention, using Fo Erhadefa, including 1) reagent and finger
Show agent prepare, 2) preparation of samples, 3) titration and 4) calculating process, it is characterised in that: the concentration of the silver nitrate solution between
Between 0.1mol/l~0.2mol/l.
The method of chloride content determination in aluminium wastewater of the present invention, using Fo Erhadefa, including 1) reagent and finger
Show agent prepare, 2) preparation of samples, 3) titration and 4) calculating process, it is characterised in that: the concentration of the nitric acid solution between 1+1~
Between 1+4.
The method of chloride content determination in aluminium wastewater of the present invention, using Fo Erhadefa, including 1) reagent and finger
Show agent preparation, 2) preparation of samples, 3) titration and 4) calculating process, it is characterised in that: the concentration of the ammonium thiocyanate standard solution
For 0.1mol/L.
The method of chloride content determination in aluminium wastewater of the present invention, measurement is accurate, easy to operate, time-consuming shorter, has
Effect eliminates aluminum ions influence in water sample, the water sample big suitable for aluminium element content, especially suitable for cannot be direct with silver nitrate
The chlorine element of titration detects.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.
Embodiment 1
The unknown chlorinity water sample of aluminium content 3.50%.
Silver nitrate solution is prepared: being weighed 17g silver nitrate (A.R) and is dissolved in the dissolution of 1000ml distilled water, constant volume obtains
The silver nitrate solution of 0.1mol/l is placed in spare in brown reagent bottle；
1+4 nitric acid solution is prepared: being measured 100ml nitric acid with graduated cylinder, is slowly injected into 400ml distilled water, it is cold to mix sealing placement
But spare to room temperature；
The ammonium thiocyanate standard solution that concentration is 0.1mol/L is prepared: being weighed 7.9g ammonium thiocyanate, is dissolved in 1000ml water, shakes
It is even, it is demarcated according to method as defined in GB/T9725-2007, concentration 0.1006mol/l；
Water sample to be measured is filtered with middling speed quantitative filter paper；Weighing 0.2g(and be accurate to 0.0001g) processed water sample to be measured is added and holds
Measuring bottle accurately pipettes 25.0ml silver nitrate solution with pipette and is added in volumetric flask, adds 5ml 1+4 nitric acid solution, 1ml sulphur
Sour iron ammonium indicator shakes up, and is titrated to the obvious brick-red precipitating of appearance, consumption with the ammonium thiocyanate standard solution of 0.1006mol/l
The volume of ammonium thiocyanate standard solution be denoted as V1, parallel to repeat five groups；
Water sample to be measured is substituted with 0.2g distilled water, repeats aforesaid operations, the ammonium thiocyanate standard solution volume of consumption is denoted as V0；
The chlorinity of test data and each group calculated separately by formula (1) is listed in table 1, relative standard deviation RSD (%) 1.73%.
Table 1
Embodiment 2
1.52% sodium chloride standard specimen 1.00mL is added in the water sample to be measured of embodiment 1, surveys chloride ion content.
Prepare and demarcate 1.52% sodium chloride solution.Ammonium thiocyanate is used after excessive silver nitrate solution is added in water sample
The silver ion of overtitration.
The nitric acid solution of 0.2mol/l silver nitrate solution and 1+2 is prepared respectively；
The preparation of ammonium thiocyanate standard solution is simultaneously demarcated as in the first embodiment, concentration 0.1006mol/l
Water sample pretreatment to be measured is the same as embodiment one；
It weighs pretreatment water sample 0.2g to be measured and is accurate to 0.0001g, 1.52% chlorination sodium standard solution 1.00g is added；Use liquid relief
Pipe accurately pipettes 25.0ml silver nitrate solution, and the nitric acid solution of 5ml 1+2 is added, and 1ml ammonium ferric sulfate indicator is added to shake up, and uses
The ammonium thiocyanate standard solution of 0.1006mol/l is titrated to the obvious brick-red precipitating of appearance, the ammonium thiocyanate standard solution of consumption
Volume be denoted as V1, parallel to repeat five groups；
Pretreatment water sample to be measured is replaced with 2g distilled water, repeats aforesaid operations, the ammonium thiocyanate standard solution measured in volume of consumption
For V0；
Test data, the chlorinity of each group calculated separately by formula (1) and recovery of standard addition are listed in table 2, and sample recovery rate exists
Between 95%-105%, accuracy is good.
Table 2
Embodiment 3
A kind of water sample of unknown chlorinity.
The configuration and preparation of standard solution are as in the first embodiment, ammonium thiocyanate concentration of standard solution 0.1012mol/l；Silver nitrate
Solution concentration 0.15mol/l；1+1 nitric acid solution.
By the test process of embodiment one, water sample 0.2g is accurately weighed, it is accurate that 25.00ml silver nitrate solution is added, it is added 1
+ 1 nitric acid 5ml, 1ml ammonium ferric sulfate indicator is titrated with the ammonium thiocyanate standard solution of 0.1012mol/l, is repeated four times, disappears
The volume of the ammonium thiocyanate standard solution of consumption is denoted as V1；
Water sample to be measured is substituted with 0.2g distilled water, repeats aforesaid operations, the ammonium thiocyanate standard solution volume of consumption is denoted as V0；
The chlorinity of test data and each group calculated separately by formula (1) is listed in table 3, relative standard deviation RSD (%) 0.14%:
Table 3
Claims (5)
1. a kind of method of chloride content determination in aluminium wastewater, using Fo Erhadefa, including 1), reagent and indicator prepare, 2)
Preparation of samples, 3) titration and 4) calculating process, it is characterised in that:
Reagent and indicator prepare: the reagent includes silver nitrate solution, nitric acid solution and ammonium thiocyanate standard solution；Ferric sulfate
Ammonium indicator；
Preparation of samples: using distilled water as blank；Water sample to be measured is filtered through middling speed quantitative filter paper；
3) titrate: including sample titration and blank titration: under identical strong acidic condition, respectively to blank and water sample to be measured into
Row titration, the ammonium thiocyanate standard solution volume of consumption are denoted as V respectively0And V1；
4) calculate: the chlorinity x of sample calculates as follows:
In formula: C --- ammonium thiocyanate concentration of standard solution, mol/l；
V0--- the ammonium thiocyanate volume of reference sample consumption, ml；
V1--- the ammonium thiocyanate volume of sample consumption, ml；
M --- sample to be tested quality, %wt.
2. the method for chloride content determination in aluminium wastewater according to claim 1, it is characterised in that: the silver nitrate solution
Concentration between 0.1mol/l~0.2mol/l.
3. the method for chloride content determination according to claim 1 or in aluminium wastewater described in 2 any one, it is characterised in that: institute
The concentration of nitric acid solution is stated between 1+1~1+4.
4. the method for chloride content determination according to claim 1 or in aluminium wastewater described in 2 any one, it is characterised in that: institute
The concentration for stating ammonium thiocyanate standard solution is 0.1mol/L.
5. the method for chloride content determination in aluminium wastewater according to claim 3, it is characterised in that: the ammonium thiocyanate mark
The concentration of quasi- solution is 0.1mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112345691A (en) * | 2020-12-07 | 2021-02-09 | 武汉海斯普林科技发展有限公司 | Method for detecting content of chloride ions in electrolyte solute of aluminum electrolytic capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106770240A (en) * | 2016-12-14 | 2017-05-31 | 四川中核艾瑞特工程检测有限公司 | A kind of cement determination of chloride ion titration outfit and titration method |
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| 张允诚等: "《电镀手册》", 31 January 2007, 国防工业出版社 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112345691A (en) * | 2020-12-07 | 2021-02-09 | 武汉海斯普林科技发展有限公司 | Method for detecting content of chloride ions in electrolyte solute of aluminum electrolytic capacitor |
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