CN107917986A - A kind of method of content using ion-chromatographic determination technical grade sodium acetate - Google Patents
A kind of method of content using ion-chromatographic determination technical grade sodium acetate Download PDFInfo
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- CN107917986A CN107917986A CN201711135217.3A CN201711135217A CN107917986A CN 107917986 A CN107917986 A CN 107917986A CN 201711135217 A CN201711135217 A CN 201711135217A CN 107917986 A CN107917986 A CN 107917986A
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- sodium acetate
- acetate
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
Abstract
The invention discloses a kind of method of the content using ion-chromatographic determination technical grade sodium acetate, it includes the following steps:(1) elution stock solution is prepared;(2) prepare elution and use liquid;(3) sodium acetate Standard Reserving Solution is prepared;(4) prepare sodium acetate and use liquid;(5) standard curve is drawn using the chromatography of ions;(6) sample is measured using the chromatography of ions;(7) sample acetate concentration calculates;(8) sample rate calculates;(9) sodium acetate content calculation in sample;The present invention has analyze speed fast, and accuracy rate is high, and complicated body influences the features such as small to it, is applicable in the conventional determining of general industry enterprise.
Description
Technical field
The present invention relates to a kind of method of the content using ion-chromatographic determination technical grade sodium acetate.
Background technology
Sodium acetate is widely used to weave as a kind of chemical industry preparation, the every field such as wastewater treatment.Enterprise is often
Need to be used by market purchase technical grade sodium acetate solution, but to the content of sodium acetate in the sodium acetate solution of purchase
Require, it is therefore desirable to which the acetic acid sodium content of the sodium acetate solution of purchase is measured.
The existing measure for technical grade sodium acetate is generally reacted using acid base titration, using phenolphthalein as indicator hydroxide
Sodium back titration simultaneously calculates acetic acid sodium content.This method refers to cumbersome, and complicated collective is disturbed easily in by sample.
The another content also having using water phase potentiometric determination anhydrous sodium acetate, complexity of this method for technical grade
The measure of body acetic acid sodium content does not apply to simultaneously.National standard to the measure of anhydrous sodium acetate, sample need to be carbonized and with HCl into
Row titration, time-consuming for this method sample treatment, and error is big.
In view of industry at present does not have the measure of technical grade acetic acid sodium content corresponding national standard, the present invention is using a kind of new
Method measures industrial acetic sodium, and it is short to have the advantages that data accurately take.
The content of the invention
The invention mainly solves the technical problem of providing a kind of accurate, the time-consuming utilization ion-chromatographic determination work of data
The method of the content of industry level sodium acetate.
Technical solution is used by the present invention solves its technical problem:One kind utilizes ion-chromatographic determination technical grade
The method of the content of sodium acetate, it includes the following steps:
(1) elution stock solution is prepared:Sodium carbonate liquor is mixed with sodium bicarbonate solution, forms elution stock solution;
(2) prepare elution and use liquid:Elution stock solution in step (1) is diluted to form elution use with deionized water
Liquid;
(3) sodium acetate Standard Reserving Solution is prepared:Anhydrous sodium acetate is dissolved in water, and adds 10.00mL elution stock solutions, is used
Water is diluted to graticule, this solution is per milli acetate ion containing 1.000mg;
(4) prepare sodium acetate and use liquid:Sodium acetate Standard Reserving Solution is diluted with deionized water and to form sodium acetate and uses liquid;
(5) standard curve is drawn using the chromatography of ions:Sodium acetate in step (4) is dense using five differences of liquid configuration
The standard liquid of degree, measures its peak height or peak area, using peak height or peak area as ordinate, with ion concentration (mg/L) for abscissa,
The regression equation of calibration curve is calculated to least square method, draws standard curve, it is the oblique of regression equation to calculate b and a, b
Rate, a are the intercept of regression equation;
(6) sample is measured using the chromatography of ions:1ml sodium acetate solutions to be measured are pipetted to 1000ml volumetric flasks
Once fixed capacity, after take the 5ml dilutions after first time constant volume to second of constant volume of 100ml volumetric flasks;Sodium acetate to be measured is molten at this time
Liquid has diluted 20000 times, and the peak height drawn after its sample introduction or peak area are checked in compared with the standard curve in step (5)
Acetate ion concentration in sample after dilution;
(7) sample acetate concentration calculates:Reagent blank is done with deionized water, it is dense to measure acetate to be measured according to formula
Degree, formula are X0 (mg/L)=[(h-h0-a) × 20000]/b, in formula:X0 is acetate concentration mg/L, and h is the peak height of sample
(or peak area), h0 are blank peak peak height (or peak area) measured value, and b is the slope of regression equation, and a is cutting for regression equation
Away from 20000 be extension rate;
(8) sample rate calculates:The sodium acetate solution to be measured of first time constant volume in step (6) is taken into 5ml into measuring cup,
Its quality (m) is surveyed with a ten thousandth balance, the density of sodium acetate, ρ are gone out according to formula scalesSodium acetate(g/L)=m × 1000/5;
(9) sodium acetate content calculation in sample:
Acetic acid sodium content, sodium acetate %=[(X are finally calculated according to formula0×82×10-3)/(59* ρ)] × 100%, formula
In:X0It is acid group concentration mg/L for second, 82 be sodium acetate molecular weight, and 59 be acetate molecular weight, and ρ is sodium acetate density.
Preferably, in step (1), the concentration of sodium carbonate liquor is 0.24 (mol/L), and the concentration of sodium bicarbonate solution is
0.3(mol/L)。
Preferably, the idiographic flow of step (1) is:Accurately weigh 25.44g sodium carbonate and 25.20g sodium acid carbonates are dissolved in
Water, is settled to 1000mL, and filtering, is stored in vinyon bottle, and refrigerator preserves.
Preferably, in step (2), elute and obtained for 100 times by the dilution of elution stock solution using liquid.
Preferably, 1.390g anhydrous sodium acetates are dissolved in water in the idiographic flow of step (3), move into 1000mL volumetric flasks
In, 10.00mL elution stock solutions are added, are diluted with water to graticule, this solution is per milli acetate ion containing 1.000mg.
Preferably, the sodium acetate Standard Reserving Solution that step (3) obtains is stored in vinyon bottle, and is put into refrigerator
In.
Preferably, the sodium acetate in step (4) dilutes 50 times by sodium acetate Standard Reserving Solution using liquid and is formed.
Preferably, the concentration of five standard liquids in step (5) is followed successively by 2mg/L, 4mg/L, 6mg/L, 9mg/L, 12mg/L.
Compared with prior art, the invention has the advantages that:Using containing for this method measure technical grade sodium acetate
Amount, has analyze speed fast, and accuracy rate is high, and complicated body influences the features such as small to it, is applicable in the routine of general industry enterprise
Measure.
Embodiment
The present invention mainly utilizes ion-chromatographic determination acetato-, is separated using ion exchange principle.By pressing down
Device processed suppresses leacheate, and background correction conductance, is then measured using electric conductivity detector.By the guarantor of the appearance of acetate anion
Time and peak height (or peak area) is stayed to carry out qualitative and quantitative acetate ion.Directly into ion chromatography after 20000 times of sample dilution
Measure its acetate concentration, after be scaled sodium acetate concentration.Sodium acetate density is measured indirectly, calculates sodium acetate percentage composition.
The instrument used has ion chromatograph, has electric conductivity detector;Chromatographic column;Anion separation column and anion
Guard column;Suppressor;Miillpore filter;Deionized water;A ten thousandth balance;Fat tripe pipette.
Technical solution is used by the present invention solves its technical problem:One kind utilizes ion-chromatographic determination technical grade
The method of the content of sodium acetate, it includes the following steps:
(1) elution stock solution is prepared:Sodium carbonate 25.44g is mixed with sodium acid carbonate 25.20g and is dissolved in water, is settled to
1000ml, by filtering, is stored in vinyon bottle and forms elution stock solution.Wherein, sodium carbonate, sodium acid carbonate are excellent
Pure level, and 2h is dried at 105 DEG C.
(2) prepare elution and use liquid:Elution stock solution is diluted into 100 times of formation elution with deionized water and uses liquid.
(3) sodium acetate Standard Reserving Solution is prepared:By 1.390g anhydrous sodium acetates, water is dissolved in, is moved into 1000mL volumetric flasks,
10.00mL elution stock solutions are added, graticule is diluted with water to, is stored in vinyon bottle and placed in refrigerator and protected
Deposit, this solution is per milli acetate ion containing 1.000mg.Above-mentioned anhydrous sodium acetate is excellent pure level, and in 105 DEG C of drying
2h。
(4) prepare sodium acetate and use liquid:Sodium acetate Standard Reserving Solution is diluted 50 times of formation sodium acetates with deionized water makes
Use liquid;
(5) standard curve is drawn using the chromatography of ions:Sodium acetate in step (4) is dense using five differences of liquid configuration
The standard liquid of degree, is respectively 2mg/L, 4mg/L, 6mg/L, 9mg/L, 12mg/), its peak height or peak area of each standard liquid are measured, with
Peak height or peak area are ordinate, and with ion concentration (mg/L) for abscissa, returning for calibration curve is calculated to least square method
Return equation, draw standard curve, draw the slope of b and a, b for regression equation, a is the intercept of regression equation.
(6) sample is measured using the chromatography of ions:1ml sodium acetate solutions to be measured are pipetted to 1000ml volumetric flasks
Once fixed capacity, after take the 5ml dilutions after first time constant volume to second of constant volume of 100ml volumetric flasks;Sodium acetate to be measured is molten at this time
Liquid has diluted 20000 times, and the peak height drawn after its sample introduction or peak area are checked in compared with the standard curve in step (5)
Acetate ion concentration in sample after dilution.
(7) sample acetate concentration calculates:Reagent blank is done with deionized water, it is dense to measure acetate to be measured according to formula
Degree, formula are X0 (mg/L)=[(h-h0-a) × 20000]/b, in formula:X0 is acetate concentration mg/L, and h is the peak height of sample
(or peak area), h0 are blank peak peak height (or peak area) measured value, and b is the slope of regression equation, and a is cutting for regression equation
Away from 20000 be extension rate.
(8) sample rate calculates:The sodium acetate solution to be measured of first time constant volume in step (6) is taken into 5ml into measuring cup,
Its quality (m) is surveyed with a ten thousandth balance, the density of sodium acetate, ρ are gone out according to formula scalesSodium acetate(g/L)=m × 1000/5.
(9) sodium acetate content calculation in sample:
Acetic acid sodium content, sodium acetate %=[(X are finally calculated according to formula0×82×10-3)/(59* ρ)] × 100%, formula
In:X0It is acid group concentration mg/L for second, 82 be sodium acetate molecular weight, and 59 be acetate molecular weight, and ρ is sodium acetate density.
According to the content of above-mentioned determination of experimental method technical grade sodium acetate, the sample of 3 batches is sampled, parallel determination 5 times, is tied
Fruit see the table below, and 3 RSD measured of batch sample 5 times are between 0.078%~0.404.
Claims (8)
1. a kind of method of content using ion-chromatographic determination technical grade sodium acetate, it includes the following steps:
(1) elution stock solution is prepared:Sodium carbonate liquor is mixed with sodium bicarbonate solution, forms elution stock solution;
(2) prepare elution and use liquid:Elution stock solution in step (1) is diluted to be formed to elute with deionized water and uses liquid;
(3) sodium acetate Standard Reserving Solution is prepared:Anhydrous sodium acetate is dissolved in water, and adds 10.00mL elution stock solutions, it is dilute with water
Release to graticule, this solution is per milli acetate ion containing 1.000mg;
(4) prepare sodium acetate and use liquid:Sodium acetate Standard Reserving Solution is diluted with deionized water and to form sodium acetate and uses liquid;
(5) standard curve is drawn using the chromatography of ions:Sodium acetate in step (4) is used into liquid five various concentrations of configuration
Standard liquid, measures its peak height or peak area, using peak height or peak area as ordinate, with ion concentration (mg/L) for abscissa, to
Least square method calculates the regression equation of calibration curve, draws standard curve, draws the slope of b and a, b for regression equation, a
For the intercept of regression equation;
(6) sample is measured using the chromatography of ions:1ml sodium acetate solutions to be measured are pipetted to 1000ml volumetric flasks first time
Constant volume, after take the 5ml dilutions after first time constant volume to second of constant volume of 100ml volumetric flasks;Sodium acetate solution to be measured has been at this time
20000 times of dilution, dilution is checked in by the peak height drawn after its sample introduction or peak area compared with the standard curve in step (5)
Acetate ion concentration in sample afterwards;
(7) sample acetate concentration calculates:Reagent blank is done with deionized water, acetate concentration to be measured is measured according to formula, it is public
Formula is X0 (mg/L)=[(h-h0-a) × 20000]/b, in formula:X0 is acetate concentration mg/L, and h is peak height (or the peak of sample
Area), h0 is blank peak peak height (or peak area) measured value, and b is the slope of regression equation, and a is the intercept of regression equation,
20000 be extension rate;
(8) sample rate calculates:The sodium acetate solution to be measured of first time constant volume in step (6) is taken into 5ml into measuring cup, with ten thousand
/ mono- balance surveys its quality (m), and the density of sodium acetate, ρ are gone out according to formula scalesSodium acetate(g/L)=m × 1000/5;
(9) sodium acetate content calculation in sample:
Acetic acid sodium content in sample, sodium acetate %=[(X are finally calculated according to formula0×82×10-3)/(59* ρ)] × 100%,
In formula:X0It is acid group concentration mg/L for second, 82 be sodium acetate molecular weight, and 59 be acetate molecular weight, and ρ is sodium acetate density.
2. a kind of method of content using ion-chromatographic determination technical grade sodium acetate as claimed in claim 1, its feature
It is:In step (1), the concentration of sodium carbonate liquor is 0.24 (mol/L), and the concentration of sodium bicarbonate solution is 0.3 (mol/L).
3. a kind of method of content using ion-chromatographic determination technical grade sodium acetate as claimed in claim 2, its feature
It is:The idiographic flow of step (1) is:Accurately weigh 25.44g sodium carbonate and 25.20g sodium acid carbonates are dissolved in water, be settled to
1000mL, filtering, is stored in vinyon bottle, and refrigerator preserves.
4. a kind of method of content using ion-chromatographic determination technical grade sodium acetate as claimed in claim 1, its feature
It is:In step (2), elute and obtained for 100 times by the dilution of elution stock solution using liquid.
5. a kind of method of content using ion-chromatographic determination technical grade sodium acetate as claimed in claim 1, its feature
It is:By 1.390g anhydrous sodium acetates in the idiographic flow of step (3), water is dissolved in, is moved into 1000mL volumetric flasks, is added
10.00mL elutes stock solution, is diluted with water to graticule, this solution is per milli acetate ion containing 1.000mg.
6. a kind of method of content using ion-chromatographic determination technical grade sodium acetate as claimed in claim 4, its feature
It is:The sodium acetate Standard Reserving Solution that step (3) obtains is stored in vinyon bottle, and is put into refrigerator.
7. a kind of method of content using ion-chromatographic determination technical grade sodium acetate as claimed in claim 1, its feature
It is:Sodium acetate in step (4) dilutes 50 times by sodium acetate Standard Reserving Solution using liquid and is formed.
8. a kind of method of content using ion-chromatographic determination technical grade sodium acetate as claimed in claim 1, its feature
It is:The concentration of five standard liquids in step (5) is followed successively by 2mg/L, 4mg/L, 6mg/L, 9mg/L, 12mg/L.
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Cited By (7)
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CN108896699A (en) * | 2018-07-06 | 2018-11-27 | 北京城市排水集团有限责任公司 | The detection method of sodium acetate in a kind of sewage |
CN111537635A (en) * | 2020-05-11 | 2020-08-14 | 成都市科隆化学品有限公司 | Method for accurately preparing acetic acid standard curve solution and detecting protected amino acid acetic acid |
CN113340834A (en) * | 2021-06-11 | 2021-09-03 | 成都市排水有限责任公司 | Method for rapidly determining content of sodium acetate in industrial-grade sodium acetate solution |
CN113358639A (en) * | 2021-06-15 | 2021-09-07 | 山东大学 | Method for detecting acetate content based on enzyme-linked color development method and application thereof |
CN113484443A (en) * | 2021-07-27 | 2021-10-08 | 西安热工研究院有限公司 | Method for testing content of impurity cations in ammonia water reagent for power plant feed water treatment |
CN113820418A (en) * | 2021-09-23 | 2021-12-21 | 浙江方圆检测集团股份有限公司 | Method for determining content of sodium acetate and 8 inorganic anions of water treatment agent |
CN114152692A (en) * | 2021-11-29 | 2022-03-08 | 成都市排水有限责任公司 | Method for simultaneously measuring industrial-grade sodium acetate and citric acid by ion chromatography |
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CN108896699A (en) * | 2018-07-06 | 2018-11-27 | 北京城市排水集团有限责任公司 | The detection method of sodium acetate in a kind of sewage |
CN111537635A (en) * | 2020-05-11 | 2020-08-14 | 成都市科隆化学品有限公司 | Method for accurately preparing acetic acid standard curve solution and detecting protected amino acid acetic acid |
CN113340834A (en) * | 2021-06-11 | 2021-09-03 | 成都市排水有限责任公司 | Method for rapidly determining content of sodium acetate in industrial-grade sodium acetate solution |
CN113340834B (en) * | 2021-06-11 | 2023-05-16 | 成都市排水有限责任公司 | Method for rapidly determining sodium acetate content in industrial sodium acetate solution |
CN113358639A (en) * | 2021-06-15 | 2021-09-07 | 山东大学 | Method for detecting acetate content based on enzyme-linked color development method and application thereof |
CN113358639B (en) * | 2021-06-15 | 2022-06-21 | 山东大学 | Method for detecting acetate content based on enzyme-linked color development method and application thereof |
CN113484443A (en) * | 2021-07-27 | 2021-10-08 | 西安热工研究院有限公司 | Method for testing content of impurity cations in ammonia water reagent for power plant feed water treatment |
CN113820418A (en) * | 2021-09-23 | 2021-12-21 | 浙江方圆检测集团股份有限公司 | Method for determining content of sodium acetate and 8 inorganic anions of water treatment agent |
CN114152692A (en) * | 2021-11-29 | 2022-03-08 | 成都市排水有限责任公司 | Method for simultaneously measuring industrial-grade sodium acetate and citric acid by ion chromatography |
CN114152692B (en) * | 2021-11-29 | 2024-03-19 | 成都市排水有限责任公司 | Method for simultaneously measuring industrial sodium acetate and citric acid by ion chromatography |
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