CN104165888A - Method for determining content of sodium chlorate in industrial alkali liquor - Google Patents
Method for determining content of sodium chlorate in industrial alkali liquor Download PDFInfo
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- CN104165888A CN104165888A CN201410397362.9A CN201410397362A CN104165888A CN 104165888 A CN104165888 A CN 104165888A CN 201410397362 A CN201410397362 A CN 201410397362A CN 104165888 A CN104165888 A CN 104165888A
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Abstract
The invention discloses a method for determining the content of sodium chlorate in industrial alkali liquor, in particular to a color indicator method based on the fact that methyl orange changes color according to the content of sodium chlorate in acidized industrial alkali liquor. The method utilizes the principle that methyl orange is orange red in acidized industrial alkali liquor, and is oxidized to fade if a strong oxidant, sodium chlorate, exists in industrial alkali liquor. The color reaction is intuitive, and the determination is easy and convenient. The determination can be performed with a conventional instrument and without the need of special preparation, and the method is worth of generalization.
Description
Technical field
The invention belongs to chemical analysis and quality inspection field, relate to a kind of process, be specifically related to the assay method of sodium chlorate content in a kind of industrial alkali liquid.
Background technology
The object of industrial alkali liquid sodium chlorate assay is by easy method, to detect the content of sodium chlorate in industrial alkali liquid, is examined the requirement whether industrial alkali liquid quality meets standard GB/T/T 11199-2006 < < high purity sodium hydroxide > > to determine.
In the table 1 of GB/T 11199-2006 < < high purity sodium hydroxide > >, listed 9 quality index of high purity sodium hydroxide, wherein the 6th is that sodium chlorate is (with NaClO
3count), and stipulated that in several specification NaOH, sodium chlorate content is respectively 0.001～0.005% (massfraction).In GB/T 11199-2006 < < high purity sodium hydroxide > >, the mensuration of 6.8 clear and definite sodium chlorate content is pressed the method for the mensuration ortho-tolidine spectrophotometric method > > regulation of the industrial NaOH sodium chlorate of GB/T 11200.1 < < content.The ultimate principle of the method is: in strong acid media, sodium chlorate is decomposed into chlorine and chlorine dioxide, under pH<1.3 condition, chlorine and chlorine dioxide react with ortho-tolidine and generate stable yellow complex, use spectrophotometric determination absorbance.The method relates to top grade pure hydrochloric acid, sodium hydroxide solution (400g/L), sodium chlorate standard solution (1g/L), sodium chlorate standard solution (10mg/L), five kinds of reagent such as ortho-tolidine indicator solution (1g/L), and separating funnel, twoport flask (500mL), water-bath (controlled in (50 ± 2) ℃), the instruments such as spectrophotometer, and working curve is drawn and sample solution is measured process more complicated, common laboratory will be carried out this mensuration, must be equipped with special instrument, medicine, and laboratory personnel is carried out to specific aim training, loaded down with trivial details in view of sodium chlorate assay, when being chosen in mensuration industrial alkali liquid, some laboratories ignore this project, for sodium chlorate content, there is the production run of strict demand to bury potential safety hazard thus.
Summary of the invention
In order to solve the deficiencies in the prior art, the invention provides the assay method of sodium chlorate content in industrial alkali liquid, utilized methyl orange to be orange red in the industrial alkali liquid of acidifying, if having strong oxidizer in industrial alkali liquid is sodium chlorate, the oxidized and principle of fading of methyl orange, color reaction is directly perceived, measure easy, and the instrument of required use is general conventional instrument, do not need to do special preparation and can implement to measure, be worthy to be popularized.
To achieve these goals, the technical solution adopted in the present invention is:
In industrial alkali liquid, the assay method of sodium chlorate content, is characterized in that, described method is for utilizing methyl orange to change the color indicator method of color according to the content of sodium chlorate in the industrial alkali liquid of acidifying.
In aforesaid industrial alkali liquid, the assay method of sodium chlorate content, is characterized in that, said method comprising the steps of:
Step 1), configuration indicator methyl orange solution;
Step 2), preparation 10mol/L NaOH mother liquor;
Step 3), preparation 1.0g/L sodium chlorate mother liquor;
Step 4), measuring NaOH mother liquor and sodium chlorate mother liquor is placed in volumetric flask and obtains mixed liquor;
Step 5), in step 4) basis on complete the preparation of series standard working solution, described series standard working solution is for to step 4) in mixed liquor add hydrochloric acid solution to make;
Step 6), with methyl orange solution titration series standard operation solution, record titration results;
Step 7), according to step 6) result drawing standard curve;
The sampling of industrial alkali liquid step 8), to be detected, acidifying and dilution;
Step 9), with methyl orange solution titration acidifying the industrial alkali liquid that diluted, record titration results;
Step 10), by typical curve, determine sodium chlorate content in industrial alkali liquid to be detected.
In aforesaid industrial alkali liquid, the assay method of sodium chlorate content, is characterized in that, described method is specially,
Step 1), configuration indicator methyl orange solution: the mass percent of preferable methyl orange solution is 0.1%, 0.1% is the mass percent of the conventional methyl orange in laboratory, mass percent is too high or too low, the time that arrives titration end-point during titration will be too fast or excessively slow, it is unfavorable for the accurate and time of experiment, to control, therefore generally take 0.1% mass percent as preferred, configuration quality number percent is that the concrete steps of 0.1% methyl orange solution are dissolved in 1000mL water for taking 1.000g methyl orange, and shaking up and obtaining mass percent is 0.1% methyl orange solution;
In this step, can carry out the configuration that mass percent is 0.1% methyl orange solution by two kinds of modes, a kind of for directly choosing the large beaker of 1000mL, after cleaning up, in beaker, inject 1000mL water, take 1.000g methyl orange soluble in water, being stirred to methyl orange dissolves completely, can be standby, another kind be first small beaker as the beaker of 200mL in injected water, then taking 1.000g methyl orange is dissolved in beaker, stir, methyl orange solution after dissolving is transferred in the volumetric flask of 1000mL, repeat above-mentioned steps, until methyl orange is all dissolved, add water to again volumetric flask scale, shake up standby.Wherein first method is more simple and quick.Methyl orange in this step can or be analyzed pure methyl orange for the pure methyl orange of top grade, is generally and analyzes pure methyl orange.
Step 2), preparation 10mol/L NaOH mother liquor: take 400.0g NaOH, soluble in water, generally be dissolved in 600mL water, realize dissolution of sodium hydroxide, lysed sodium hydroxide solution is transferred in 1L volumetric flask, be diluted with water to scale, shake up and obtain NaOH mother liquor;
In this step, NaOH can or be analyzed pure cerium hydroxide sodium for top grade pure cerium hydroxide sodium, preferably top grade pure cerium hydroxide sodium.
Step 3), the sodium chlorate mother liquor of preparation 1.0g/L: take 1.000g sodium chlorate, be dissolved in water in beaker, lysed sodium chlorate solution is transferred in 1L volumetric flask, be diluted with water to scale, shake up and obtain sodium chlorate mother liquor; In this step, sodium chlorate can for the pure sodium chlorate of top grade or be analyzed pure sodium chlorate, the pure sodium chlorate of general analysis.
Step 4), measuring NaOH mother liquor and sodium chlorate mother liquor is placed in volumetric flask and obtains mixed liquor: at 11 100mL volumetric flasks, put into respectively 10mL step 2) the NaOH mother liquor of preparation, successively get again 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL, 6.0mL, 7.0mL, 8.0mL, 9.0mL, 10.0mL step 3) in the sodium chlorate mother liquor of preparation put into respectively 11 volumetric flasks, shake up;
Step 5), in step 4) basis on complete the preparation of series standard working solution, described series standard working solution is for to step 4) in mixed liquor add hydrochloric acid solution to make: draw 20mL hydrochloric acid solution and add respectively step 4) in 11 volumetric flasks in, be diluted with water to scale, shake up, be mixed with series standard working solution;
Step 6), with methyl orange solution titration series standard operation solution, record titration results: by step 5) in series standard working solution pour into respectively in 11 conical flasks, each conical flask is splashed into step 1 gradually) methyl orange solution carry out titration, until series standard working solution be orange red and 30 seconds in do not disappear, record the methyl orange solution consumption V1 that each conical flask is corresponding, unit is mL; In this step, series standard working solution is all poured in corresponding conical flask, can not only be poured into a part, directly pour into, conventionally adopt 500ml conical flask.
Step 7), according to step 6) result drawing standard curve: with the sodium chlorate content ω in 11 conical flasks
1methyl orange solution consumption V for ordinate, correspondence
1for horizontal ordinate production standard curve;
Step 8), the sampling of industrial alkali liquid to be detected, acidifying and dilution: get 10mL industrial alkali liquid to be measured and put into 100mL conical flask, add the acidifying of 20mL hydrochloric acid solution, and be diluted with water to scale, shake up standby;
Step 9), with methyl orange solution titration acidifying the industrial alkali liquid that diluted, record titration results: to step 8) in conical flask acidifying the industrial alkali liquid that diluted splash into gradually step 1) methyl orange solution carry out titration, until industrial alkali liquid be orange red and 30 seconds in do not disappear, record methyl orange consumption V
2;
Step 10), by typical curve, determine sodium chlorate content in industrial alkali liquid to be detected: in step 7) locate V on the horizontal ordinate of the typical curve made
2, pass through V
2work is perpendicular to the perpendicular line of horizontal ordinate, and the intersection point of perpendicular line and typical curve is T, and the ordinate that T is ordered is the sodium chlorate content ω in industrial alkali liquid
2.
The assay method of sodium chlorate content in aforesaid industrial alkali liquid, it is characterized in that, the water of using in described method is the laboratory water that meets secondary water specification in GB/T 6682-2008 < < assay laboratory's water specification and test method > >, uses the method for repeatedly distillation and ion-exchange to produce and obtains.
The assay method of sodium chlorate content in aforesaid industrial alkali liquid, it is characterized in that, the step 7 of described method) in, in 11 conical flasks, density of sodium chlorate is respectively 0mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L, 5.0mg/L, 6.0mg/L, 7.0mg/L, 8.0mg/L, 9.0mg/L, 10.0mg/L, and corresponding density is 1.43g/cm
340% high alkali liquid in sodium chlorate content ω
1be respectively 0%, 0.0007%, 0.0014%, 0.0021%, 0.0028%, 0.0035%, 0.0042%, 0.0049%, 0.0056%, 0.0063%, 0.007%.
In aforesaid industrial alkali liquid, the assay method of sodium chlorate content, is characterized in that, the step 8 of described method), step 9) in, the sampling of industrial alkali liquid, acidifying, dilution and titration operation complete in 30min.
The assay method of sodium chlorate content in aforesaid industrial alkali liquid, it is characterized in that, the step 6 of described method), step 9) in, the methyl orange solution that preferably service property (quality) number percent is 0.1% carries out titration, mass percent is that 0.1% methyl orange solution rate of titration is 1 drop/sec, the volume of 1 solution is approximately 0.04mL, often splash into the methyl orange solution that 1 mass percent is 0.1%, shake conical flask 3s, and observe in conical flask the change color of test solution and take and judge whether to continue to drip the methyl orange solution that mass percent is 0.1%, finally should control drop hangs and does not fall, with conical flask inwall, drop is come on the lower, with wash bottle purge conical flask inwall, shake up, repeat aforesaid operations until the test solution in conical flask be orange red and 30 seconds in do not disappear.
The assay method of sodium chlorate content in aforesaid industrial alkali liquid, it is characterized in that, the step 5 of described method), step 8) in, described hydrochloric acid solution is top grade pure hydrochloric acid solution, i.e. step 5), step 8) in hydrochloric acid solution used be the hydrochloric acid solution of oxygen-free voltinism material.
Beneficial effect of the present invention is: the assay method of sodium chlorate content in industrial alkali liquid provided by the invention, by drawing standard curve, locate the content of sodium chlorate in actual industrial alkali lye, from typical curve, in the consumption of known methyl orange and industrial alkali liquid, sodium chlorate content is in linear relation, the consumption that is methyl orange has reacted the content of sodium chlorate in industrial alkali liquid, directly perceived and simple.The method has utilized methyl orange to be orange red in the industrial alkali liquid of acidifying, if having strong oxidizer in industrial alkali liquid is sodium chlorate, oxidized and the principle of fading of methyl orange, color reaction is directly perceived, measures easyly, and the instrument of required use is general conventional instrument, methyl orange indicator is also the chemical reagent of common laboratory indispensability, therefore this assay method does not need to do special preparation and can implement to measure, quick and easy, is worthy to be popularized.
Accompanying drawing explanation
Fig. 1 is the methyl orange metachromatic principle figure of the assay method of sodium chlorate content in industrial alkali liquid of the present invention;
Fig. 2 is that sodium chlorate content-mass percent is the typical curve of 0.1% methyl orange solution consumption;
Fig. 3 is definite figure of sodium chlorate content in industrial alkali liquid.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is done to concrete introduction.The raw material adopting in the application, comprises that methyl orange, NaOH, sodium chlorate, hydrochloric acid solution and industrial alkali liquid are commercial, without specific (special) requirements.The present embodiment is applied with certain generating plant 660MW supercritical thermal power unit the example that is determined as that method of the present invention carries out and is introduced.
Certain generating plant has the coal-fired Turbo-generator Set of two 660MW, and between water treatment vehicle, technological process is: former water → pre-service → cation bed → decarbonizer → anion bed → mixed bed.Wherein, Zeo-karb is housed in cation bed, anion exchange resins is housed in anion bed, cationic, anionic exchange resin is housed in mixed bed.After National Day in 2013, after this disposal system anion bed regeneration, put into operation, occur that water outlet quality worsens phenomenon.By analysis, doubtful anion bed in regenerative process anion exchange resins by due to alkali liquor oxidized degraded.Because it is one-level ionic membrane caustic soda that this generating plant requires the alkali lye of supplier's supply, and because sodium chlorate project assay method is loaded down with trivial details, so only done three projects such as naoh concentration, di-iron trioxide and sodium chloride content in 9 quality index of high purity sodium hydroxide that in GB/T 11199-2006 < < high purity sodium hydroxide > >, table 1 is listed when the quality inspection of alkali lye arrival is checked and accepted, do not chemically examined sodium chlorate content.In order to make a definite diagnosis culprit, this factory extracts " ionic membrane caustic soda " sample of storing in alkali tank, adopts method of the present invention, its sodium chlorate content is detected to the equal severe overweight of result proof sodium chlorate content.In industrial alkali liquid of the present invention, as shown in Figure 1, specific implementation method is as follows for the methyl orange metachromatic principle figure of the assay method of sodium chlorate content.
Step 1), the methyl orange solution that configuration quality number percent is 0.1%: with analytical balance, take 0.1000g and analyze pure methyl orange, get after 100mL beaker cleans up and be filled to scale, the pure methyl orange of the analysis taking is soluble in water, stir standby;
Step 2), preparation 10mol/L NaOH mother liquor: take 400.0g with counter balance and analyze pure cerium hydroxide sodium, be dissolved in 600mL water, lysed sodium hydroxide solution is transferred in 1L volumetric flask, be diluted with water to scale, shake up and obtain NaOH mother liquor;
Step 3), the sodium chlorate mother liquor of preparation 1.0g/L: take 1.0000g with analytical balance and analyze pure sodium chlorate, be dissolved in water in beaker, lysed sodium chlorate solution is transferred in 1L volumetric flask, be diluted with water to scale, shake up and obtain sodium chlorate mother liquor;
Step 4), measuring NaOH mother liquor and sodium chlorate mother liquor is placed in volumetric flask and obtains mixed liquor: at 11 100mL volumetric flasks, put into respectively 10mL step 2) the NaOH mother liquor of preparation, successively get again 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL, 6.0mL, 7.0mL, 8.0mL, 9.0mL, 10.0mL step 3) in the sodium chlorate mother liquor of preparation put into respectively 11 volumetric flasks, shake up;
Step 5), in step 4) basis on complete the preparation of series standard working solution, described series standard working solution is for to step 4) in mixed liquor add hydrochloric acid solution to make: draw 20mL top grade pure hydrochloric acid solution and add respectively step 4) in 11 volumetric flasks in, be diluted with water to one by one scale, shake up, be mixed with series standard working solution.Wherein, in 11 conical flasks, density of sodium chlorate is respectively 0mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L, 5.0mg/L, 6.0mg/L, 7.0mg/L, 8.0mg/L, 9.0mg/L, 10.0mg/L, and in the concentrated base of corresponding undiluted mistake, (40% industrial alkali liquid density is pressed 1.43g/cm to sodium chlorate concentration expressed in percentage by weight
3meter) be respectively 0%, 0.0007%, 0.0014%, 0.0021%, 0.0028%, 0.0035%, 0.0042%, 0.0049%, 0.0056%, 0.0063%, 0.007%, be the content (ω of sodium chlorate in high alkali liquid
1, ν %);
Step 6), the methyl orange solution titration series standard operation solution that is 0.1% by mass percent, record result: by step 5) in series standard working solution pour into respectively in 11 conical flasks, with 1mL transfer pipet, respectively each conical flask is slowly splashed into step 1) mass percent be 0.1% methyl orange solution carries out titration, mass percent is that 0.1% methyl orange solution rate of titration is 1 drop/sec, often splash into the methyl orange solution that 1 mass percent is 0.1%, shake conical flask 3s, and observe in conical flask the change color of test solution and take and judge whether to continue to drip the methyl orange solution that mass percent is 0.1%, finally controlling drop hangs and does not fall, with conical flask inwall, drop is come on the lower, with wash bottle purge conical flask inwall, shake up, repeat aforesaid operations until the test solution in conical flask is in orange red and 30s does not disappear, record the methyl orange solution consumption V1 that each conical flask is corresponding, the methyl orange solution volume consuming is respectively 0.04mL, 0.09mL, 0.14mL, 0.19mL, 0.24mL, 0.29mL, 0.33mL, 0.38mL, 0.43mL, 0.48mL, 0.53mL,
Step 7), according to step 6) result drawing standard curve: with the sodium chlorate content ω in 11 conical flasks
1(ν %) is the methyl orange solution consumption V that ordinate, corresponding mass percent are 0.1%
1(mL) be horizontal ordinate production standard curve, as shown in Figure 2, figure neutral line related coefficient is 0.9999;
Step 8), the sampling of industrial alkali liquid to be detected, acidifying and dilution: get 10mL ionic membrane caustic soda to be measured and put into 100mL conical flask, add the acidifying of 20mL top grade pure hydrochloric acid, and be diluted with water to scale, shake up standbyly, be about to ionic membrane caustic soda and be diluted to original 10 times, concentration is about 1mol/L;
Step 9), the methyl orange solution titration acidifying that is 0.1% by mass percent the industrial alkali liquid diluting: to step 8) in conical flask acidifying the ionic membrane caustic soda that diluted splash into gradually step 1) mass percent be 0.1% methyl orange solution carries out titration, mass percent is that 0.1% methyl orange solution rate of titration is 1 drop/sec, often splash into the methyl orange solution that 1 mass percent is 0.1%, shake conical flask 3s, and observe in conical flask the change color of test solution and take and judge whether to continue to drip the methyl orange solution that mass percent is 0.1%, finally controlling drop hangs and does not fall, with conical flask inwall, drop is come on the lower, with wash bottle purge conical flask inwall, shake up, repeat aforesaid operations until the test solution in conical flask is in orange red and 30s does not disappear, record methyl orange consumption V
2, be 0.48mL, the methyl orange solution volume consuming is 0.48mL, step 8) and step 9) in 30min, complete,
Step 10), by typical curve, determine sodium chlorate content in industrial alkali liquid: in step 7) locate V on the horizontal ordinate of the typical curve made
2, pass through V
2work is perpendicular to the perpendicular line of horizontal ordinate, and the intersection point of perpendicular line and typical curve is T, and the ordinate that T is ordered is the sodium chlorate content ω in ionic membrane caustic soda
2reading is 0.0063%, as shown in Figure 3, the sodium chlorate content's index of HL-I (NaOH 45%) high-class product and Grade A is respectively sodium chlorate (with NaClO and in GB/T11199-2006 < < high purity sodium hydroxide > > table 1
3meter)≤0.002%, sodium chlorate are (with NaClO
3meter)≤0.003%, therefore, the sodium chlorate content severe overweight in this ionic membrane caustic soda.The assay method of this kind of sodium chlorate content is fast and simple, and the reagent using is that laboratory is conventional standby, and measurement result is reliable, is applicable to the Fast Measurement to sodium chlorate content in industrial alkali liquid.
The water of using in the method is the laboratory water that meets secondary water specification in GB/T 6682-2008 < < assay laboratory's water specification and test method > >, use the method for repeatedly distillation and ion-exchange to produce and obtain, and the method at room temperature.
More than show and described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand, and above-described embodiment does not limit the present invention in any form, and all employings are equal to replaces or technical scheme that the mode of equivalent transformation obtains, all drops in protection scope of the present invention.
Claims (8)
1. the assay method of sodium chlorate content in industrial alkali liquid, is characterized in that, described method is for utilizing methyl orange to change the color indicator method of color according to the content of sodium chlorate in the industrial alkali liquid of acidifying.
2. the assay method of sodium chlorate content in industrial alkali liquid according to claim 1, is characterized in that, said method comprising the steps of:
Step 1), configuration indicator methyl orange solution;
Step 2), preparation 10mol/L NaOH mother liquor;
Step 3), preparation 1.0g/L sodium chlorate mother liquor;
Step 4), measuring NaOH mother liquor and sodium chlorate mother liquor is placed in volumetric flask and obtains mixed liquor;
Step 5), in step 4) basis on complete the preparation of series standard working solution, described series standard working solution is for to step 4) in mixed liquor add hydrochloric acid solution to make;
Step 6), with methyl orange solution titration series standard operation solution, record titration results;
Step 7), according to step 6) result drawing standard curve;
The sampling of industrial alkali liquid step 8), to be detected, acidifying and dilution;
Step 9), with methyl orange solution titration acidifying the industrial alkali liquid that diluted, record titration results;
Step 10), by typical curve, determine sodium chlorate content in industrial alkali liquid to be detected.
3. the assay method of sodium chlorate content in industrial alkali liquid according to claim 2, it is characterized in that, described method is specially, step 1), configuration indicator methyl orange solution: the mass percent of preferable methyl orange solution is 0.1%, configuration quality number percent is that the step of 0.1% methyl orange solution is dissolved in 1000mL water for taking 1.000g methyl orange, and shaking up and obtaining mass percent is 0.1% methyl orange solution;
Step 2), preparation 10mol/L NaOH mother liquor: take 400.0g NaOH, soluble in water, lysed sodium hydroxide solution is transferred in 1L volumetric flask, be diluted with water to scale, shake up and obtain NaOH mother liquor;
Step 3), the sodium chlorate mother liquor of preparation 1.0g/L: take 1.000g sodium chlorate, be dissolved in water in beaker, lysed sodium chlorate solution is transferred in 1L volumetric flask, be diluted with water to scale, shake up and obtain sodium chlorate mother liquor;
Step 4), measuring NaOH mother liquor and sodium chlorate mother liquor is placed in volumetric flask and obtains mixed liquor: at 11 100mL volumetric flasks, put into respectively 10mL step 2) the NaOH mother liquor of preparation, successively get again 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL, 6.0mL, 7.0mL, 8.0mL, 9.0mL, 10.0mL step 3) in the sodium chlorate mother liquor of preparation put into respectively 11 volumetric flasks, shake up;
Step 5), in step 4) basis on complete the preparation of series standard working solution, described series standard working solution is for to step 4) in mixed liquor add hydrochloric acid solution to make: draw 20mL hydrochloric acid solution and add respectively step 4) in 11 volumetric flasks in, be diluted with water to scale, shake up, be mixed with series standard working solution;
Step 6), with methyl orange solution titration series standard operation solution: by step 5) in series standard working solution pour into respectively in 11 conical flasks, each conical flask is splashed into step 1 gradually) methyl orange solution carry out titration, until series standard working solution be orange red and 30 seconds in do not disappear, record the methyl orange solution consumption V1 that each conical flask is corresponding;
Step 7), drawing standard curve: with the sodium chlorate content ω in 11 conical flasks
1methyl orange solution consumption V for ordinate, correspondence
1for horizontal ordinate production standard curve;
Step 8), the sampling of industrial alkali liquid to be detected, acidifying and dilution: get 10mL industrial alkali liquid to be detected and put into 100mL conical flask, add the acidifying of 20mL hydrochloric acid solution, and be diluted with water to scale, shake up standby;
Step 9), with methyl orange solution titration acidifying the industrial alkali liquid that diluted: to step 8) in conical flask acidifying the industrial alkali liquid that diluted splash into gradually step 1) methyl orange solution carry out titration, until industrial alkali liquid be orange red and 30 seconds in do not disappear, record methyl orange consumption V
2;
Step 10), by typical curve, determine sodium chlorate content in industrial alkali liquid to be detected: in step 7) locate V on the horizontal ordinate of the typical curve made
2, pass through V
2work is perpendicular to the perpendicular line of horizontal ordinate, and the intersection point of perpendicular line and typical curve is T, and the ordinate that T is ordered is the sodium chlorate content ω in industrial alkali liquid
2.
4. the assay method of sodium chlorate content in industrial alkali liquid according to claim 3, it is characterized in that, the water of using in described method is the laboratory water that meets secondary water specification in GB/T 6682-2008 < < assay laboratory's water specification and test method > >, uses the method repeat distillation and ion-exchange to produce and obtains.
5. the assay method of sodium chlorate content in industrial alkali liquid according to claim 3, it is characterized in that, the step 7 of described method) in, in 11 conical flasks, density of sodium chlorate is respectively 0mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L, 5.0mg/L, 6.0mg/L, 7.0mg/L, 8.0mg/L, 9.0mg/L, 10.0mg/L, and corresponding density is 1.43g/cm
340% high alkali liquid in sodium chlorate content ω
1be respectively 0%, 0.0007%, 0.0014%, 0.0021%, 0.0028%, 0.0035%, 0.0042%, 0.0049%, 0.0056%, 0.0063%, 0.007%.
6. the assay method of sodium chlorate content in industrial alkali liquid according to claim 3, is characterized in that the step 8 of described method), step 9) in, the sampling of industrial alkali liquid, acidifying, dilution and titration operation complete in 30min.
7. the assay method of sodium chlorate content in industrial alkali liquid according to claim 3, it is characterized in that, the step 6 of described method), step 9) in, the methyl orange solution that preferably service property (quality) number percent is 0.1% carries out titration, mass percent is that 0.1% methyl orange solution rate of titration is 1 drop/sec, often splash into the methyl orange solution that 1 mass percent is 0.1%, shake conical flask 3s, and observe in conical flask the change color of test solution and take and judge whether to continue to drip the methyl orange solution that mass percent is 0.1%, finally controlling drop hangs and does not fall, with conical flask inwall, drop is come on the lower, with wash bottle purge conical flask inwall, shake up, repeat aforesaid operations until the test solution in conical flask be orange red and 30 seconds in do not disappear.
8. the assay method of sodium chlorate content in industrial alkali liquid according to claim 3, is characterized in that the step 5 of described method), step 8) in, described hydrochloric acid solution is top grade pure hydrochloric acid solution.
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| CN109580605A (en) * | 2018-12-04 | 2019-04-05 | 攀枝花钢企欣宇化工有限公司 | The measuring method of sodium chlorate in sodium hydroxide solution |
| CN110794084A (en) * | 2019-11-19 | 2020-02-14 | 攀枝花钢企欣宇化工有限公司 | Method for measuring calcium chlorate content |
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