CN101576481B - Method for measuring contents of anionic surface active substances by methylene blue spectrometry - Google Patents
Method for measuring contents of anionic surface active substances by methylene blue spectrometry Download PDFInfo
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- CN101576481B CN101576481B CN2009100218848A CN200910021884A CN101576481B CN 101576481 B CN101576481 B CN 101576481B CN 2009100218848 A CN2009100218848 A CN 2009100218848A CN 200910021884 A CN200910021884 A CN 200910021884A CN 101576481 B CN101576481 B CN 101576481B
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Abstract
The invention discloses a method for measuring contents of anionic surface active substances in alkali metal salts, alkaline-earth metal salts or alkaline-earth metal hydroxides by a methylene blue spectrometry, which comprises the following steps: using nitric acid water solution to dissolve out the anionic surface active substances in the solid alkali metal salts, and preparing 0.1 to 0.5 mol/Lsolution; adding methylene blue solution into the solution, adjusting the pH of the solution to between 4.6 and 5.0 by using acetic acid and sodium acetate buffer solution; measuring the absorbency of the solution by a spectral photometer; after the absorbency A of the solution is deducted from blank absorbency Ao, forming a linear relation with the content of a complex compound formed by the reaction of the anionic surface active substances and the methylene blue in the solution; and obtaining the contents of the anionic surface active substances in the solution through a standard curve, and then obtaining the contents of the anionic surface active substances in the solid alkali metal salts, the alkaline-earth metal salts or the alkaline-earth metal hydroxides through conversion. The experimental cost of the analysis method is low, the analysis operation is simple, and the repeatability of the analysis result is good.
Description
Technical field
The invention belongs to the chemical analysis technology field; The method that relates to contents of anionic surface active substances in a kind of oxyhydroxide that adopts metric measurement alkali metal salt, alkali salt and earth alkali metal relates in particular to the method for contents of anionic surface active substances in the oxyhydroxide of a kind of methylene blue spectrophotometry solid alkali metal salt, alkali salt or earth alkali metal.
Background technology
In the preparation process of the oxyhydroxide of solid alkali metal salt, alkali salt or earth alkali metal; State of aggregation and surface nature for crystallization control process, product pattern and size-grade distribution, product; Often in the preparation system, add adjuvant; The adjuvant that uses is main with surface reactive material, in the product that obtains, often contains certain quantity of additive, in order to regulate and control preparation process and product quality; The crystallization mechanism of understanding alkali metal salt, alkali salt or alkaline earth metal hydroxide under the adjuvant effect needs the accurate content of measuring adjuvant (especially surface reactive material adjuvant) in the product.
Spectrophotometry for anionic surface active substances in the environmental water sample has had some bibliographical informations, and the principle of its method mostly is to utilize kation developer and anionic surface active substances generation associated reaction.Difference according to assay method can be divided into two types with it: the direct development process of extraction spectrophotometric method and water.Extraction spectrophotometric method is to utilize kation developer and anionic surface active substances generation associated reaction at first to generate associated matter, associated matter is extracted under the visible region specific wavelength, measures absorbance after the organic phase then.Mensuration to anionic surface active substances among the standard GB 7494-37 is exactly extraction earlier, measures with AAS then, but this kind method operation relative complex, and mostly extractant is noxious material.There are problems such as mensuration system poor stability, disturbing factor are many in the direct development process of water.
Above-mentioned two kinds of methods mainly are the mensuration to contents of anionic surface active substances in environmental water sample, potable water, the sanitary sewage.In solid alkali metal salt, alkali salt or the oxyhydroxide, and the mensuration of contents of anionic surface active substances in the alkaline metal, alkaline-earth metal ions solution, owing to receive the restriction of salinity, and the influence of interfering ion, existing analytical approach can not adopt.Also there is not at present a kind of method of maturation to be suitable for the mensuration of contents of anionic surface active substances in the oxyhydroxide of solid alkali metal salt, alkali salt or earth alkali metal.
Summary of the invention
The method that the purpose of this invention is to provide contents of anionic surface active substances in the oxyhydroxide of a kind of methylene blue spectrophotometry alkali metal salt, alkali salt or earth alkali metal.
The method of contents of anionic surface active substances in the oxyhydroxide of methylene blue spectrophotometry alkali metal salt of the present invention, alkali salt or earth alkali metal; Be earlier with the anionic surface active substances in the oxyhydroxide of aqueous solution of nitric acid stripping solid alkali metal salt, alkali salt or the earth alkali metal of mass concentration 35～70%, be mixed with the solution that concentration is 0.1～0.5mol/L; In solution, adding concentration is 0.05～0.1g/L methylene blue solution, and making the methylene blue and the ratio of the amount of substance of anionic surface active substances to be measured is 4: 1～1: 1; And with the pH value of acetic acid-sodium acetate buffer solution regulator solution between 4.6～5.0; Use the spectrophotometric determination solution absorbency; Solution absorbency A deduction blank absorbency A
o(blank absorbency A
oAbsorbance for the methylene blue solution of the hydroxide solution of the alkali metal salt, alkali salt or the earth alkali metal that do not contain anionic surface active substances) after, the content of the complex compound that forms with anionic surface active substances in the solution and methylene blue is linear; In the 0-0.05g/L scope, set up the linear relation equation of absorbance and complex compound content; Obtain the content of anionic surface active substances in the solution through typical curve, obtain contents of anionic surface active substances in solid alkali metal salt, alkali salt or the alkaline earth metal hydroxide through conversion again.
The preparation of said methylene blue solution:, be mixed with the methylene blue solution that concentration is 0.05～0.1g/L with the dissolve with ethanol of methylene blue with mass concentration 20～50%.
The preparation of said acetic acid-sodium acetate buffer solution: with sodium acetate water dissolving, be mixed with the solution that concentration is 1.0～2.0mol/L after, regulate pH value to 4.6～5.0 with glacial acetic acid again, promptly get damping fluid.
The mensuration wavelength of said absorbance is 200～900nm.
The drafting of said typical curve:
(1) gets the volumetric flask of 6 25mL; Add the alkaline metal that do not contain anionic surface active substances and the alkaline-earth metal salt solution 4mL of concentration respectively at 0.1～0.5mol/L; Add 0,0.5,1.0,1.5,2.0 then successively, the concentration of 2.5mL is the anionic surface active substances solution of 0～0.05g/L, the buffer solution 2mL of pH value between 4.6～5.0, the methylene blue solution 4mL that concentration is 0.05～0.1g/L, constant volume; Shake up, place 2～7 minutes to be measured;
(2) with the standard solution of above-mentioned preparation content order from low to high, its absorbance of sequentially determining according to anionic surface active substances; Solution absorbency A deduction blank absorbency A
oAfter, the content of the complex compound that forms with anionic surface active substances in the solution and methylene blue is linear; Set up the linear relation equation of absorbance and complex compound content, i.e. typical curve.
Contents of anionic surface active substances in the oxyhydroxide of said solid alkali metal, alkali salt or earth alkali metal obtains through the following formula conversion:
The content of C---the anionic surface active substances that obtains from typical curve, the mg/L of unit
The volume of V---solution to be measured, Unit
12.5---liquor capacity conversion multiple in the experimentation
The initial weight of M---solid sample, the g of unit
X---the content of anionic surface active substances in the solid sample, the mg/g of unit
The blank absorbency value of this experiment is less, but when calculating contents of anionic surface active substances, the absorbance of sample still will be deducted blank absorbency, otherwise can bring deviation to the result who measures.
Said alkaline metal is lithium, sodium, potassium; Earth alkali metal is magnesium, calcium, strontium, barium; Alkali metal salt is lithium halide, magnesium halide, potassium halide, lithium carbonate, sodium carbonate, sal tartari, lithium sulfate, sodium sulphate, glazier's salt; Alkali salt is magnesium halide, calcium halide, barium halide, halogenation strontium, magnesium carbonate, lime carbonate, barium carbonate, strontium carbonate, basic magnesium carbonate, magnesium sulphate, calcium sulphate, barium sulphate, strontium sulfate; The oxyhydroxide of earth alkali metal is magnesium hydroxide, calcium hydroxide, strontium hydroxide, baryta hydrate.
Said anionic surface active substances is carboxylate R-COONa, sulfuric acid R-OSO
3Na, sulphonate R-SO
3Na, phosphate ester salt R-OPO
3Na
2(R is an organic group), Potassium Hydrogen Phthalate.
The present invention also is suitable for the mensuration of contents of anionic surface active substances in alkaline metal and the alkaline-earth metal ions solution.
The present invention compared with prior art has following good effect:
1, analytical approach of the present invention, cost is low, and analytic process is simple and quick, and analysis result accuracy is high, favorable reproducibility, can solve the technical matters that contents of anionic surface active substances is difficult to measure in present alkaline metal and alkali salt or the oxyhydroxide.
2, Li
+, Na
+, K
+, Mg
2+, Ca
2+, Sr
2+, Ba
2+, Br
-, Cl
-, I
-, HPO
4 2-, H
2PO
4 -, Ac
-, NO
3 -Isoionic existence does not all produce interference to measuring, and in addition, the existence of Triton-100, Tween-80, isopropyl alcohol etc. more helps the stable of solution absorbance.
3, absorbance is stable within a certain period of time for methylene blue solution and methylene blue-anionic surface active substances mixed solution.
4, the methylene blue developer is cheap and easy to get, and its related solution is easy to preparation, does not receive the interference of human factor.
Description of drawings
Fig. 1 is the spectral scan curve that contains the related solution of lauryl sodium sulfate
1---the methylene blue solution of basic magnesium carbonate (is done reference with distilled water, corresponding A
0)
2---contain the methylene blue solution (doing reference with distilled water, corresponding A) of the basic magnesium carbonate of lauryl sodium sulfate
3---the methylene blue solution that contains the basic magnesium carbonate of lauryl sodium sulfate (is done reference with reagent blank, corresponding A-A
0, reagent blank promptly obtains the solution of curve 1)
Fig. 2 is the spectral scan curve that contains the related solution of Potassium Hydrogen Phthalate
1---the methylene blue solution of basic magnesium carbonate (is done reference with distilled water, corresponding A
0)
2---contain the methylene blue solution (doing reference with distilled water, corresponding A) of the basic magnesium carbonate of Potassium Hydrogen Phthalate
3---the methylene blue solution that contains the basic magnesium carbonate of Potassium Hydrogen Phthalate (is done reference with reagent blank, corresponding A-A
0, reagent blank promptly obtains the solution of curve 1)
Fig. 3 is the typical curve of embodiment 1
Fig. 4 is the typical curve of embodiment 2
Embodiment
The content of lauryl sodium sulfate in embodiment one, the mensuration basic magnesium carbonate
1, instrument and vessel
Volumetric flask 25mL, 50mL
Graduated cylinder 10mL
Balance range 220g, sensibility reciprocal 0.1mg
Acidometer precision ± 0.01
Ultraviolet-visible spectrophotometer luminosity accuracy ± 0.002Abs
2, reagent
The methylene blue reagent analysis is pure
Lauryl sodium sulfate is analyzed pure
Sodium acetate is analyzed pure
Glacial acetic acid is analyzed pure
Ethanol is analyzed pure
3, experimental procedure
(1) dissolve appearance: accurately take by weighing the basic magnesium carbonate that does not contain lauryl sodium sulfate and contain each 2.5649g of basic magnesium carbonate sample of lauryl sodium sulfate, the quality error of two samples is controlled in the 0.2mg.Aqueous solution of nitric acid with 35% concentration dissolves appearance, dissolves the appearance process and in airtight container, carries out, and is mixed with the solution that the basic carbonate magnesium density is 0.129mol/L.
(2) preparation of acetic acid-sodium-acetate buffer: get sodium acetate 5.4g, add water 50mL and make its dissolving, regulate pH value to 4.6 with glacial acetic acid, thin up is to 100mL again, promptly gets the pH value and be acetic acid-sodium acetate buffer solution of 4.6.
(3) preparation of methylene blue solution: take by weighing methylene blue 0.0211g, dissolve with 20-50% ethanol, be transferred to then in the 250mL volumetric flask, add the water constant volume, getting concentration is the methylene blue solution of 0.0844g/L.
(4) preparation of sodium dodecyl sulfate solution: take by weighing the 0.1015g lauryl sodium sulfate, use dissolved in distilled water, be transferred in the 200mL volumetric flask, constant volume obtains the solution that concentration is 0.5072g/L.
(5) measure wavelength determination: 1 in volumetric flask getting 25mL; The basic carbonate magnesium solution 4mL that to add the above-mentioned concentration that does not contain lauryl sodium sulfate successively in the volumetric flask be 0.129mol/L, concentration is the methylene blue solution 4mL of 0.0844g/L, concentration is the lauryl sodium sulfate 2mL of 0.5072g/L; The pH value is above-mentioned acetic acid-sodium acetate buffer solution 2mL of 4.6; Constant volume shakes up then, and the range of wavelengths at 200～900nm after static 4 minutes carries out spectral scan, and the result sees Fig. 1.
Visible by Fig. 1, the solution absorbency value there are differences in wavelength 666nm place, can utilize this difference, measures the content of lauryl sodium sulfate in the basic magnesium carbonate with calibration curve method.Therefore, measuring wavelength confirms at 666nm.
(6) preparation of standard solution: 5 in volumetric flask getting 25mL; The basic carbonate magnesium solution 4mL that in each volumetric flask, respectively to add the above-mentioned concentration that does not contain lauryl sodium sulfate be 0.129mol/L, above-mentioned concentration is the methylene blue solution 4mL of 0.0844g/L, adds 0.5,1.0,1.5,2.0 then successively, the concentration for preparing of 2.5mL is the sodium dodecyl sulfate solution of 0.5072g/L; The pH value is 4.6 buffer solution 2mL; Be settled to 25mL at last, shake up, obtain standard solution.
(7) drafting of typical curve: the standard solution placement after 4 minutes, in 666nm wavelength bioassay standard solution absorbency value, is obtained the typical curve equation:
A
abs＝-0.00319C+0.00085(C：mg/L)，(R＝0.9980)
A
Abs---standard model solution absorbency A deduction blank absorbency A
oDifference
The content of C---lauryl sodium sulfate, unit: mg/L
(8) preparation of testing sample solution: 1 in volumetric flask getting 25mL; Adding the above-mentioned concentration that contains lauryl sodium sulfate is 0.129mol/L basic carbonate magnesium solution 4mL; Concentration is the methylene blue solution 4mL of 0.0844g/L, and the pH value is acetic acid-sodium acetate buffer solution 2mL of 4.6, is settled to 25mL at last; Shake up, obtain solution to be measured;
(9) calculating of lauryl sodium sulfate content in the testing sample solution: after above-mentioned testing sample solution placement 4 minutes, measure absorbance in the 666nm wavelength.Obtain the content of lauryl sodium sulfate in the testing sample solution through typical curve: be 5.1120mg/L
(10) cubage of lauryl sodium sulfate in the solid basic magnesium carbonate: calculate by following formula:
The content of C---the lauryl sodium sulfate that obtains from typical curve, 5.1120mg/L
The volume of V---obtain solution, 25mL
12.5---liquor capacity conversion multiple in the experimentation
2.5649---the weight of basic magnesium carbonate sample, the g of unit
X---the content of lauryl sodium sulfate in the solid basic magnesium carbonate, the mg/g of unit
Through calculating, the content that records lauryl sodium sulfate in the present embodiment solid basic magnesium carbonate is 0.0498mg/g, and relative standard deviation is 0.53%, and the recovery is 98.7%.
The assay of Potassium Hydrogen Phthalate in embodiment 2, the basic magnesium carbonate
1, instrument and vessel
Identical with embodiment 1
2, reagent
With Potassium Hydrogen Phthalate (benchmark) replacement, other is identical with embodiment 1 with lauryl sodium sulfate.
3, experimental procedure
(1) dissolve appearance: each 2.5649g of basic magnesium carbonate sample that accurately takes by weighing the basic magnesium carbonate that does not contain Potassium Hydrogen Phthalate and contain Potassium Hydrogen Phthalate, the quality error of two samples is controlled in the 0.2mg.Aqueous solution of nitric acid with 35% dissolves appearance, dissolves the appearance process and in airtight container, carries out, and is mixed with the solution that concentration is 0.129mol/L.
(2) preparation of acetic acid-sodium-acetate buffer: same with embodiment 1.
(3) preparation of methylene blue solution: same with embodiment 1.
(4) preparation of Potassium Hydrogen Phthalate: take by weighing Potassium Hydrogen Phthalate 0.1021g, use dissolved in distilled water, be transferred in the 200mL volumetric flask, constant volume obtains the solution that concentration is 0.5102g/L.
(5) measure wavelength determination: 1 in volumetric flask getting 25mL; Adding the concentration that does not contain Potassium Hydrogen Phthalate successively in the volumetric flask is the basic carbonate magnesium solution 4mL of 0.129mol/L, and concentration is 0.0844g/L methylene blue solution 4mL, and concentration is the Potassium Hydrogen Phthalate solution 2mL of 0.5102g/L; PH is acetic acid-sodium acetate buffer solution 2mL of 4.6; Constant volume shakes up, and leaves standstill that the range of wavelengths at 200～900nm carries out spectral scan after 4 minutes, and the result sees Fig. 2.Visible by Fig. 2, there is significant difference in the solution absorbency value in wavelength 332 nm places, can utilize this difference, measures the content of Potassium Hydrogen Phthalate in the basic magnesium carbonate with calibration curve method.Therefore, measuring wavelength confirms at 332nm.
(6) preparation of standard solution: 6 in volumetric flask getting 25mL; In each volumetric flask, respectively adding above-mentioned no Potassium Hydrogen Phthalate concentration is 0.129mol/L basic carbonate magnesium solution 4mL, and concentration is the methylene blue solution 4mL of 0.0844g/L, adds 0,0.5,1.0,1.5,2.0 then successively, the concentration for preparing of 2.5mL is the Potassium Hydrogen Phthalate solution of 0.5102g/L; The pH value is acetic acid-sodium acetate buffer solution 2mL of 4.6; Be settled to 25mL at last, shake up, obtain standard solution.
(7) drafting of typical curve: the standard solution placement after 4 minutes, is measured its absorbance at wavelength 332nm place, obtain the typical curve equation:
A
abs＝0.05366C+0.00493，R＝0.9887。
A
Abs---standard model solution absorbency A deduction blank absorbency A
oDifference
The content of C---Potassium Hydrogen Phthalate, unit: mg/L
(8) preparation of testing sample solution: 1 in volumetric flask getting 25mL; The basic carbonate magnesium solution 4mL that to add the above-mentioned concentration that contains Potassium Hydrogen Phthalate be 0.129mol/L; Concentration is the methylene blue solution 4mL of 0.0844g/L, and the pH value is acetic acid-sodium acetate buffer solution 2mL of 4.6, is settled to 25mL at last; Shake up, obtain solution to be measured.
(9) calculating of Potassium Hydrogen Phthalate content in the testing sample solution: after above-mentioned testing sample solution placement 4 minutes, measure its absorbance in the 332nm wavelength.Obtain the content of Potassium Hydrogen Phthalate in the testing sample solution through typical curve: be 0.9177mg/L
(10) calculating of Potassium Hydrogen Phthalate content in the solid basic magnesium carbonate: calculate by following formula:
The content of C---the anionic surface active substances that obtains from typical curve, 0.9177mg/L
The volume of V---obtain solution, 25mL
12.5---liquor capacity conversion multiple in the experimentation
2.5649---the weight (unit: g) of basic magnesium carbonate sample
X---the content (unit: mg/g) of Potassium Hydrogen Phthalate in the solid basic magnesium carbonate
Through calculating, the content that records Potassium Hydrogen Phthalate in the present embodiment basic magnesium carbonate is 0.0896mg/g, and standard deviation is 1.48%, and the recovery is 103%.
The assay method of contents of anionic surface active substances and embodiment 1,2 are basic identical in the oxyhydroxide of other solid alkali metal salt, alkali salt or earth alkali metal.
Claims (6)
1. the method for contents of anionic surface active substances in the oxyhydroxide of methylene blue spectrophotometry alkali metal salt, alkali salt or earth alkali metal; It is characterized in that: earlier with the anionic surface active substances in the oxyhydroxide of aqueous solution of nitric acid stripping solid alkali metal salt, alkali salt or earth alkali metal, being mixed with alkaline metal or alkaline-earth metal ions concentration is the solution of 0.1～0.5mol/L; In solution, adding concentration is 0.05～0.1g/L methylene blue solution, and making the methylene blue and the ratio of the amount of substance of anionic surface active substances to be measured is 4: 1～1: 1; And with the pH value of acetic acid-sodium acetate buffer solution regulator solution between 4.6～5.0; Use the spectrophotometric determination solution absorbency; Solution absorbency A deduction blank absorbency A
oAfter, the content of the complex compound that forms with anionic surface active substances in the solution and methylene blue is linear; Obtain the content of anionic surface active substances in the solution through typical curve, obtain contents of anionic surface active substances in the oxyhydroxide of solid alkali metal salt, alkali salt or earth alkali metal through conversion again;
The drafting of said typical curve:
(1) preparing standard solution: the volumetric flask of getting 6 25mL; Add the alkaline metal that do not contain anionic surface active substances and the alkaline-earth metal salt solution 4mL of concentration respectively at 0.1～0.5mol/L; Add 0,0.5,1.0,1.5,2.0 then successively, the concentration of 2.5mL is the anionic surface active substances solution of 0～0.05g/L, the buffer solution 2mL of pH value between 4.6～5.0, the methylene blue solution 4mL that concentration is 0.05～0.1g/L, constant volume; Shake up, place 2～7 minutes to be measured;
(2) with the standard solution of above-mentioned preparation content order from low to high, its absorbance of sequentially determining according to anionic surface active substances; Solution absorbency A deduction blank absorbency A
oAfter, the content of the complex compound that forms with anionic surface active substances in the solution and methylene blue is linear; Set up the linear relation equation of absorbance and complex compound content, i.e. typical curve;
Contents of anionic surface active substances in the oxyhydroxide of said solid alkali metal salt, alkali salt or earth alkali metal obtains through the following formula conversion:
The content of C---the anionic surface active substances that obtains from typical curve, the mg/L of unit
The volume of V---solution to be measured, Unit
12.5---liquor capacity conversion multiple in the experimentation
The initial weight of m---solid sample, the g of unit
X---the content of anionic surface active substances in the solid sample, mg/g.
2. the method for contents of anionic surface active substances in the oxyhydroxide of methylene blue spectrophotometry alkali metal salt, alkali salt or earth alkali metal according to claim 1 is characterized in that: with the anionic surface active substances in the oxyhydroxide of aqueous solution of nitric acid stripping alkali metal salt, alkali salt or the earth alkali metal of mass concentration 35～70%.
3. the method for contents of anionic surface active substances in the oxyhydroxide of methylene blue spectrophotometry alkali metal salt, alkali salt or earth alkali metal according to claim 1; It is characterized in that: the preparation of said methylene blue solution:, be mixed with the methylene blue solution that concentration is 0.05～0.1g/L the dissolve with ethanol of methylene blue with mass concentration 20～50%.
4. the method for contents of anionic surface active substances in the oxyhydroxide of methylene blue spectrophotometry alkali metal salt, alkali salt or earth alkali metal according to claim 1; It is characterized in that: the preparation of said acetic acid-sodium acetate buffer solution: the sodium acetate water is dissolved; After being mixed with the solution that concentration is 1.0～2.0mol/L; Regulate pH value to 4.6～5.0 with glacial acetic acid again, promptly get damping fluid.
5. the method for contents of anionic surface active substances in the oxyhydroxide of methylene blue spectrophotometry alkali metal salt, alkali salt or earth alkali metal according to claim 1, it is characterized in that: the mensuration wavelength of said absorbance is 200～900nm.
6. the method for contents of anionic surface active substances in methylene blue spectrophotometry alkali metal salt, alkali salt or the alkaline earth metal hydroxide according to claim 1, it is characterized in that: said anionic surface active substances is carboxylate, sulfuric acid, sulphonate, phosphate ester salt or Potassium Hydrogen Phthalate.
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