CN110736804A - Method for measuring total nitrogen content based on ion chromatography technology - Google Patents
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Abstract
The invention belongs to the field of analysis and detection, and particularly relates to a method for determining total nitrogen content based on an ion chromatography technology, which aims to solve the technical problem of providing methods for determining total nitrogen content based on the ion chromatography technology.
Description
Technical Field
The invention belongs to the field of analysis and detection, and particularly relates to a method for determining total nitrogen content based on an ion chromatography technology.
Background
In the current domestic standard, for example, "determination of total nitrogen in water quality HJ 636-.
In the prior art, methods for measuring the total nitrogen content in water by adopting an ion chromatography technology are available, but after alkaline potassium persulfate is used for digestion, hydrochloric acid is added to neutralize the system, the concentration of chloride ions is too high, which can interfere with subsequent detection, for example, the chromatographic peak of chloride ions with too high concentration can form a tailing peak in chromatographic flow, the separation degree between the chromatographic peak and a nitrate peak is reduced, so that the detection result is inaccurate, the concentration of the chloride ions can be diluted, the operation steps can be increased, and the risk of system pollution is increased.
Disclosure of Invention
The invention aims to solve the technical problem of providing methods for measuring the total nitrogen content based on the ion chromatography technology, which comprises the following steps:
A. oxidizing and digesting a system to be detected by using alkaline potassium persulfate to obtain a sample to be detected, directly detecting the sample to be detected by using ion chromatography without adding acid for neutralization, and obtaining a peak area corresponding to nitrate radical in the sample to be detected; the eluent of the ion chromatography is a system containing hydroxide radicals;
B. the method is the same as the step A except that the system to be measured is replaced by water with the same volume, and the peak area corresponding to the nitrate radical in the blank group is obtained;
C. and (6) calculating to obtain the total nitrogen content of the system to be measured according to the standard curve and the data in the step A, B.
Specifically, in the method for determining the total nitrogen content based on the ion chromatography, the system to be determined is any system requiring determination of the nitrogen content. For example: a water system with water as the main component. The aqueous system may contain alcohols, aldehydes, alkanolamines, amides, inorganic ammonium compounds, ammonium salts and/or undefined nitrogen-containing compounds, etc.
Preferably, in the method for determining total nitrogen content based on ion chromatography, the hydroxide radical-containing system is an aqueous solution of sodium hydroxide or potassium hydroxide.
, the concentration of the sodium hydroxide solution or potassium hydroxide solution is 7.5-12.5 mmol/L, preferably 10 mmol/L.
Preferably, in the above method for measuring total nitrogen content based on ion chromatography, the column of the ion chromatography is a hydrophilic anion column, and in the step , the column is SH-AC-11(250 mm. times.4.6 mm).
Preferably, in the method for measuring the total nitrogen content based on the ion chromatography, the column temperature of the ion chromatography is 35-45 ℃, and the column temperature is 35 ℃ in the step.
Preferably, in the method for determining the total nitrogen content based on the ion chromatography technology, the flow rate of the ion chromatography is 0.8-1.2 mL/min, and the flow rate of the ion chromatography is 1.1mL/min in the step.
Preferably, in the method for measuring total nitrogen content by ion chromatography, the method for preparing the standard curve comprises: measuring different amounts of NO3 -And oxidizing and digesting the standard solution by adopting alkaline potassium persulfate, detecting by adopting ion chromatography to obtain a corresponding peak area, and drawing a standard curve of the addition amount-peak area according to the addition amount and the peak area.
Specifically, in the method for determining the total nitrogen content based on the ion chromatography, the oxidation digestion is specifically performed by: and mixing the system to be detected with an alkaline potassium persulfate solution, and digesting for 30-40 min at 120 +/-5 ℃.
, the digestion temperature is 120 ℃ in the method for measuring total nitrogen content based on ion chromatography.
, the concentration of the alkaline potassium persulfate solution is 20-25 g/L, and is further performed, and the concentration of the alkaline potassium persulfate solution is 25 g/L.
Further , the oxidative digestion is carried out under sealed conditions in the method for measuring total nitrogen content based on ion chromatography, and further , the digestion is carried out by using penicillin bottles.
Specifically, in the method for measuring the total nitrogen content based on the ion chromatography technology, the concentration of sulfate radical in a sample to be measured entering an ion chromatograph is controlled to be below 1000 mg/L.
The invention provides methods for measuring total nitrogen content by using ion chromatography, which can directly detect by using ion chromatography without adding extra hydrochloric acid for neutralization after oxidizing and digesting an object to be detected and matching with a subsequent hydroxyl leaching system.
Drawings
FIG. 1 is an ion chromatogram of a "digestion solution" in a hydroxide system in test example 8;
FIG. 2 is an ion chromatogram of the "digestion solution" in the carbonate system in test example 8.
Detailed Description
The invention relates to a method for measuring total nitrogen content based on an ion chromatography technology, which comprises the following steps:
A. carrying out oxidation digestion on a system to be detected by using sufficient or excessive alkaline potassium persulfate to obtain a sample to be detected, detecting nitrate radical in the sample to be detected by adopting ion chromatography to obtain a peak area corresponding to the nitrate radical in the sample to be detected, and obtaining a detection result of the sample to be detected; the eluent of the ion chromatography is a hydroxyl system;
B. the method is the same as the step A except that the sample to be detected is replaced by distilled water with the same volume, and the corresponding peak area of nitrate radical in the blank sample group is obtained, so that the detection result of the blank group is obtained;
C. by NO3 -Standard solution, taking NO with different addition amounts3 -Oxidizing and digesting the standard solution by adopting alkaline potassium persulfate, detecting by adopting ion chromatography to obtain chromatographic peak areas corresponding to different addition amounts, and drawing an addition amount-chromatographic peak area standard curve;
D. and C, calculating to obtain the total nitrogen content of the system to be detected according to the detection result of the sample to be detected in the step A, the detection result of the blank group in the step B and the standard curve in the step C.
In the method of the present invention, the step of,the system to be tested can be any system in which the nitrogen content needs to be determined. For example: a water system with water as the main component. The aqueous system may contain alcohols, aldehydes, alkanolamines, amides, inorganic ammonium compounds, ammonium salts and/or undefined nitrogen-containing compounds, etc. For example: ethanol, triethylamine, DMF, NH4 +Ethylene glycol, diethylene glycol, DMAC, urea and/or triethanolammonium, and the like.
In the method of the present invention, in order to ensure that the oxidative digestion process does not leak, the oxidative digestion is preferably carried out under a sealed condition. Preferably, penicillin bottles are used. And (3) filling the substance into a penicillin bottle, melting and sealing the penicillin bottle, and then carrying out oxidation digestion.
In the method, because a large amount of sulfate ions formed by decomposing potassium persulfate exist in the system after oxidation and digestion, in order to protect instruments and chromatographic columns, the concentration of the sulfate ions in a sample to be detected entering an ion chromatograph cannot exceed 1000mg/L at most, and if the concentration of the sulfate ions exceeds the concentration, dilution is needed.
In the experimental examples of the present invention, the ion chromatograph used was purchased from Qingdao Han chromatography technology Limited, model CIC-D120, sodium hydroxide (analytical purity, Guangxi science and technology development Limited, Tianjin), potassium persulfate (EMSURE grade, Germany Merck), purified water (commercially available Waha purified water), deionized water (made by laboratory), 20mL penicillin bottle (commercially available), triethanolamine, NO3 -The standard (1000 mug/mL) is purchased from national analysis and test center for nonferrous metal and electronic materials.
In the test examples of the present invention, samples were treated in the following manner and detected under the ion chromatography conditions shown in table 1.
Accurately weighing a system to be measured into a 25mL volumetric flask, adding deionized water to a constant volume, taking a proper amount of a sample with the constant volume into a 20mL penicillin bottle, complementing the total volume of the sample to 10.0mL by the deionized water, adding 5.0mL of 25g/L alkaline potassium persulfate solution, and sealing. Standing at 120 deg.C for 30min, and cooling. The solution was filtered through a 0.45 μm microporous membrane and diluted 10-fold with deionized water to obtain a test solution.
TABLE 1
| Cl-、NO3 -、SO4 2- | |
| Chromatographic column | SH-AC-11 type ion chromatographic column 250mm x 4.0mm |
| Column temperature and |
35℃，1.1mL/min |
| Leacheate | 10mmol/L NaOH |
| Detector | Conductivity detector |
| Suppressor and current thereof | SHY-A-6 type 75mA |
| Volume of the quantitative ring | 25μL |
Test example 1 determination of ion chromatography leacheate
Because the mixed system to be detected adopts sufficient or excessive alkaline potassium persulfate solution for oxidation and digestion, the solution is strong alkaline, hydrochloric acid is usually added in the prior art for detection after the system is neutralized, but chloride ions are introduced, the subsequent detection is interfered due to overhigh concentration of the chloride ions, for example, a tailing peak is formed in chromatographic flow by the chromatographic peak of the chloride ions with overhigh concentration, the separation degree between the chromatographic peak and a nitrate peak is reduced, the detection result is inaccurate, the concentration of the diluted chloride ions increases the operation steps, and the risk of system pollution is increased. In order to avoid introducing new interfering ions, the inventor finds through tests and analysis that when the ion chromatography is adopted for detection, a sample to be detected can be directly leached by a strong alkaline system, namely a hydroxide system without adding hydrochloric acid for neutralization, and a good detection effect can be obtained. At this time, if a carbonate elution system is selected, the retention time of sulfate is too long, and exceeds 30min, the excessive sulfate in the digestion system has serious damage to the chromatographic column, the single analysis time is long, and due to the introduction of a strong alkaline sample in the digestion system, the change of the strength of the eluate is easily caused, so that the measurement repeatability is deteriorated.
Based on a strong alkaline leaching system, the inventor conducts optimized screening on the concentration of a leaching solution, compares elution conditions under hydroxide radical concentrations of 10mmol/L and 15mmol/L, and finds that after the concentration of the leaching solution is reduced, although the peak time of each ion is prolonged, the separation degree between different ions is increased, the interference is reduced, and particularly under the sodium hydroxide concentration of 10mmol/L, NO is reduced3 -And a large amount of SO4 2-The separation between them is better. Therefore, the concentration of the eluting solution is preferably 7.5 to 12.5 mmol/L. Most preferably, the concentration of the leacheate is 10 mmol/L.
Test example 2 measurement of System blank
The deionized water is used as a blank in the experiment, the direct sample injection of the deionized water and the sample injection after the alkaline potassium persulfate is adopted for digestion are respectively measured, the peak areas of the nitrate radicals under the two conditions are shown in the table 2.
TABLE 2 determination of System blanks
| Direct sample introduction of deionized water | Sample introduction after digestion of deionized water | |
| NO3 -Area of ion peak | 785 | 2094 |
As shown in Table 2, the peak area of the sample after digestion by deionized water is far larger than that of the sample after direct sample injection, and nitrogen compounds in the alkaline potassium persulfate solution are presumed to increase the content of nitrate in the system.
TABLE 3 continuous 6 system blank measurements and their standard deviations
| 1 | 2 | 3 | 4 | 5 | 6 | Standard deviation sigma | |
| A | 2010 | 2183 | 2151 | 2033 | 2076 | 2146 | 70.4 |
Test example 3 precision test
Under the selected ion chromatographic analysis condition, 6 20mL penicillin bottles are respectively and accurately added with quantitative NO3 -The standard solution (1000. mu.g/mL) was made up to 10.0mL by adding deionized water, 5.0mL of an alkaline potassium persulfate solution was added, and the mixture was sealed. According to the digestion and detection method, sample injection analysis is carried out, the peak area of nitrate ions is measured, and the measurement result is shown in table 4.
TABLE 4 ion chromatography for determination of nitrate-precision test
| 1 | 2 | 3 | 4 | 5 | 6 | RSD％(n＝6) | |
| A | 15855 | 16092 | 15994 | 16160 | 17554 | 16039 | 3.88 |
Test example 4 plotting of Standard Curve
7 penicillin bottles with 20mL are taken in the experiment, and NO is accurately added respectively3 -0, 100, 200, 400, 800, 1600 and 3200 mul of standard solution (the concentration is 1000 mug/mL), supplementing deionized water to 10.0mL, adding 5.0mL of alkaline potassium persulfate solution, and sealing. According to the digestion and detection method, the sample injection analysis and the NO determination are carried out3 -The peak area of the ion was measured, and the results are shown in Table 5. With NO3 -The curve obtained by linear regression with the addition (μ g) on the abscissa and the peak area on the ordinate was 162.14x-1726.30, and the correlation coefficient r was 0.9999. (wherein y represents a peak area, and x represents the nitrate content in the digestion system,. mu.g).
TABLE 5 ion chromatography determination-standard curve for nitrate
| NO3 -/μg | 0 | 100 | 200 | 400 | 800 | 1600 | 3200 |
| A | 2104 | 16092 | 31255 | 61377 | 124998 | 253424 | 520123 |
Test example 5 sample reproducibility test
The test further examines the repeatability of the sample determination, the repeatability test takes analytically pure triethanolamine as a substrate (concentration is 8.452mg/mL), 6 penicillin bottles with 20mL are respectively taken, 100 mu L of triethanolamine solution is accurately added, deionized water is used for supplementing to 10.0mL, 5.0mL of alkaline potassium persulfate solution is added, sealing is carried out, according to the digestion and detection method, sample injection analysis and NO determination are carried out3 -The peak area of the ion was measured, and the results are shown in Table 6.
TABLE 6 ion chromatography for determination-repeatability tests of nitrate
| 1 | 2 | 3 | 4 | 5 | 6 | Mean value of | RSD％(n＝6) | |
| A | 46185 | 46431 | 45403 | 46381 | 46324 | 47556 | 46380 | 1.49 |
Test example 6 recovery test
In the test, concentration analytical pure triethanolamine is used as a substrate (the concentration is 8.452mg/mL), and a standard addition recovery test with 3 concentration levels (200, 400 and 600 mu g) is designed3 -The standard solution (concentration 1000. mu.g/mL) was made up to 10.0mL with deionized water 200, 400, 600. mu.L, and 5.0mL of alkaline potassium persulfate solution was added and sealed. According to the digestion and detection method, the sample injection analysis and the NO determination are carried out3 -Peak area of ion and calculating NO from working curve3 -The content and recovery rate of ions are shown in Table 7 and Table 8, and the test results show that the triethanolamine is used as a substrate and 3 concentration levels are adoptedThe recovery rate is between 101 and 108 percent, and the method is high in accuracy.
TABLE 7 ion chromatography for nitrate determination-recovery test-1
Remarking: taking the peak area average value in the yield test back from the background value; the measured amount is the content of nitrate radical in the digestion system, mu g
TABLE 8 ion chromatography for nitrate determination-recovery test-2
Remarking: the background values were retrieved as the average of the nitrate measurements in the yield tests.
Test example 7 method detection Limit
Since it is difficult to obtain a blank digestion system without nitrate under the current experimental conditions, the method detection limit of the experiment is 3 times of the standard deviation of the blank value of the system as the method detection limit, and the calculated value is 1.3 mug, which is shown in table 9.
TABLE 9 ion chromatography for determination of nitrate-calculation of detection limits by method
| 1 | 2 | 3 | 4 | 5 | 6 | Standard deviation sigma | |
| A | 2010 | 2183 | 2151 | 2033 | 2076 | 2146 | 70.4 |
| NO3 - | 23.04 | 24.11 | 23.91 | 23.19 | 23.45 | 23.88 | 0.43 |
Test example 8
The invention compares the detection results of the same digestion solution under the conditions of adding hydrochloric acid and not adding hydrochloric acid and under the conditions of a carbonate leaching system and a hydroxyl leaching system, and the digestion solution is prepared by triethanolamine as shown in Table 10.
Remarking: calculated values were calculated based on 2. mu.g/ml and 5. mu.g/ml nitrate standard solutions.
"HCl + H" in Table 10 above2O' indicates that the system does not contain digestion solution, and hydrochloric acid is added as a hydrochloric acid blank; "digestion solution + HCl" means that the system contains digestion solution and hydrochloric acid; "digestion solution" means that the system contains digestion solution, and hydrochloric acid is not added; based on the common sense of comparison, the addition amount of the same substance in the comparison group is the same, namely the hydrochloric acid amount in different sample systems to be detected is the same, and the digestion liquid amount in different sample systems to be detected is the same.
As can be seen from Table 10, for the same digestion solution, the NaOH system is used as the eluent, the interference of HCl is eliminated, the detection results of adding hydrochloric acid and not adding hydrochloric acid are equivalent, and the method of the invention can obtain the detection effect equivalent to that of adding hydrochloric acid under the condition of not adding hydrochloric acid2CO3/NaHCO3The system is used as an eluent, the interference of HCl is eliminated, the detection results are greatly different between the detection results of adding hydrochloric acid and the detection results of not adding hydrochloric acid, meanwhile, for the digestion solution of the same , the peak area obtained by adopting a NaOH system is larger, which indicates that the NaOH system is adopted to be more than the Na system2CO3/NaHCO3The system sensitivity is higher.
The ion chromatogram of the digestion solution under a hydroxyl system is shown in figure 1, and the ion chromatogram of the digestion solution under a carbonate system is shown in figure 2; wherein 12.307min in fig. 1 is the retention time of nitrate, 13.963min in fig. 2 is the retention time of nitrate, and as can be seen from fig. 1 and 2, the use of hydroxide as the eluent has a large peak area of nitrate and long retention time intervals with other peaks, which indicates that the use of hydroxide as the eluent has the advantages of good separation degree and high sensitivity, and the use of hydroxide as the eluent has a shorter single separation time.
Claims (10)
1. The method for measuring the total nitrogen content based on the ion chromatography technology is characterized in that: the method comprises the following steps:
A. oxidizing and digesting a system to be detected by using alkaline potassium persulfate to obtain a sample to be detected, directly detecting the sample to be detected by using ion chromatography without adding acid for neutralization, and obtaining a peak area corresponding to nitrate radical in the sample to be detected; the eluent of the ion chromatography is a system containing hydroxide radicals;
B. the method is the same as the step A except that the system to be measured is replaced by water with the same volume, and the peak area corresponding to the nitrate radical in the blank group is obtained;
C. and (6) calculating to obtain the total nitrogen content of the system to be measured according to the standard curve and the data in the step A, B.
2. The method for measuring the total nitrogen content based on the ion chromatography technology as claimed in claim 1, wherein the system to be measured is any system requiring measurement of nitrogen content, and further , the system to be measured is a water system with water as a main component.
3. The method for determining the total nitrogen content based on the ion chromatography technology as claimed in claim 1 or 2, wherein the hydroxide radical system is sodium hydroxide aqueous solution or potassium hydroxide aqueous solution, the concentration of the sodium hydroxide aqueous solution or the potassium hydroxide aqueous solution is 7.5-12.5 mmol/L in the step of , and the concentration of the sodium hydroxide aqueous solution or the potassium hydroxide aqueous solution is 10mmol/L in the step of .
4. The method for measuring the total nitrogen content based on the ion chromatography technique as claimed in any one of claims 1-3 and , wherein the ion chromatography column is hydrophilic anion chromatography column, and the step is performed, and the chromatography column is SH-AC-11 type.
5. The method for measuring the total nitrogen content based on the ion chromatography technique as claimed in any one of claims 1-4, wherein the column temperature of the ion chromatography is 35-45 ℃ and the column temperature is 35 ℃ in the further steps.
6. The method for measuring the total nitrogen content based on the ion chromatography technique as claimed in any one of claims 1 to 5 and , wherein the flow rate of the ion chromatography is 0.8-1.2 mL/min, and the flow rate is 1.1mL/min in the further step.
7. The method for measuring total nitrogen content according to any one of claims 1 to 6 to , wherein the standard curve is prepared by measuring different amounts of NO3 -And oxidizing and digesting the standard solution by adopting alkaline potassium persulfate, detecting by adopting ion chromatography to obtain a corresponding peak area, and drawing a standard curve of the addition amount-peak area according to the addition amount and the peak area.
8. The method for determining the total nitrogen content based on the ion chromatography technology as claimed in any one of claims 1 to 7 to , wherein the oxidation digestion is specifically performed by mixing a system to be measured with an alkaline potassium persulfate solution and digesting for 30 to 40min at 120 ± 5 ℃.
9. The method for determining the total nitrogen content based on the ion chromatography technology as claimed in any one of claims 1 to 8 to , wherein the oxidative digestion adopts a penicillin bottle.
10. The method for determining the total nitrogen content based on the ion chromatography technique of any one of claims 1 to 9 and , wherein the concentration of sulfate radicals in the sample to be tested entering the ion chromatography is controlled to be below 1000 mg/L.
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