CN111983130A - Method for detecting complete ammonia distillation based on full-automatic Kjeldahl determination instrument color method - Google Patents
Method for detecting complete ammonia distillation based on full-automatic Kjeldahl determination instrument color method Download PDFInfo
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- CN111983130A CN111983130A CN202010926672.0A CN202010926672A CN111983130A CN 111983130 A CN111983130 A CN 111983130A CN 202010926672 A CN202010926672 A CN 202010926672A CN 111983130 A CN111983130 A CN 111983130A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/002—Determining nitrogen by transformation into ammonia, e.g. KJELDAHL method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
Abstract
The invention relates to a method for detecting complete ammonia distillation based on a full-automatic Kjeldahl apparatus color method, which comprises the following steps: putting an organic compound sample containing protein, concentrated sulfuric acid and a catalyst into a test tube to be heated and digested together, so that the protein is decomposed, decomposed ammonia radical ions and sulfate radical ions are combined to generate ammonium sulfate, then dissociating ammonia gas under the action of alkaline distillation, cooling the dissociated ammonia gas and water vapor together through a condenser pipe, and then feeding the ammonia gas and the water vapor into a titration cup filled with boric acid; dripping hydrochloric acid or sulfuric acid titration solution with known concentration into the titration cup, detecting the titration speed and recording in real time; the titration speed is gradually increased from high to low, the interval time of slow titration is gradually increased, or until no titration is carried out in unit time, the ammonia gas is judged to be completely distilled. The complete ammonia distillation is judged by detecting the titration speed in real time, so that the detection data of the Kjeldahl determination instrument are more accurate and stable and can be repeated; and the correctness of the calculated data of the sample is also made a basis.
Description
Technical Field
The invention relates to the technical field of applied chemistry, in particular to a method for detecting complete ammonia distillation based on a full-automatic Kjeldahl apparatus color method.
Background
The full-automatic Kjeldahl azotometer color method comprises the steps of adding alkali into a sample, distilling and heating the sample for a period of time to enable the sample and the alkali to generate a displacement reaction, displacing ammonia gas, flowing the ammonia gas and steam into a titration cup together through a condensation pipe, absorbing the ammonia gas by absorption liquid in the titration cup, simultaneously neutralizing the ammonia gas through titration of standard acid or standard alkali, and calculating the nitrogen content of the sample through finally measuring and consuming the volume of the standard liquid. Due to the fact that the variety of samples is various, ammonia gas of some samples can not be completely distilled in the set time, and due to the fact that people can only set the distillation time by experience, the problem that the ammonia gas can not be completely distilled exists, detection data of the Kjeldahl apparatus is deviated and inaccurate, and repeatability is poor.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for detecting the complete distillation of ammonia gas based on a full-automatic Kjeldahl azotometer color method.
Therefore, the technical scheme is that the method for detecting the complete ammonia gas distillation based on the full-automatic Kjeldahl apparatus color method comprises the following steps:
step S10: putting an organic compound sample containing protein, concentrated sulfuric acid and a catalyst into a test tube to be heated and digested together, so that the protein is decomposed, decomposed ammonia radical ions and sulfate radical ions are combined to generate ammonium sulfate, then dissociating ammonia gas under the action of alkaline distillation, cooling the dissociated ammonia gas and water vapor together through a condenser pipe to form ammonia water, and feeding the ammonia water into a titration cup filled with boric acid; step S20: dripping hydrochloric acid or sulfuric acid titration solution with known concentration into the titration cup, detecting the titration speed and recording in real time; step S30: before the distillation is finished, the titration speed is changed from high to low along with the neutralization of the ammonia gas by the standard acid, the interval time of slow dripping is gradually prolonged, or the titration is not carried out in unit time, and the ammonia gas is judged to be completely distilled.
Preferably, the step S20 further includes the step S21: the acid-base value is displayed by a color developing agent while hydrochloric acid or sulfuric acid titration liquid with known concentration is dripped into the titration cup, and the change of color is detected and recorded in real time.
Preferably, the step S20 further includes the step S22: and (3) detecting that the color developing agent in the titration cup filled with the boric acid is red, changing the color developing agent into blue after ammonia enters the titration cup, changing the color developing agent into reddish when titration is carried out to be balanced, reducing the titration speed along with less ammonia entering the titration cup generated by the distilled sample, and judging that the ammonia is completely distilled if slow drops with larger intervals exist.
Preferably, the method further comprises step S40: detecting the establishment of an analysis map of the complete ammonia distillation, setting the distillation time of a sample as an X axis, setting the titration amount as a Y axis, and extending a color frame from an original point along the X axis direction, wherein the color frame is used for representing the real-time color in the titration cup; drawing the titration speed recorded in real time into a histogram in the sample distillation time, wherein the histogram is drawn above a color frame; changes in color of the developer recorded in real time were added to the histogram and color box during the sample distillation time.
The technical scheme of the invention has the following advantages:
1. according to the method for detecting the complete ammonia distillation based on the full-automatic Kjeldahl apparatus color method, whether the ammonia is completely distilled or not is judged by detecting the titration speed and the change of the color of the sample in the ammonia distillation process in real time, so that the detection data of the Kjeldahl apparatus is more accurate and stable and can be repeated; the correctness of the calculated nitrogen content data of the sample is also based; the method has important contribution and significance for improving the accuracy of the detection items of the Kjeldahl determination instrument.
2. The method for detecting the complete ammonia distillation based on the full-automatic Kjeldahl apparatus color method establishes a real-time analysis map for detecting whether the ammonia is completely distilled based on the full-automatic Kjeldahl apparatus, can enable the detection data of the Kjeldahl apparatus to be more accurate and stable by simultaneously detecting the titration speed and the color change of the color developing agent in real time, and can enable the established analysis map for detecting the complete ammonia distillation to be more visual and intuitive by adding the color change of the color developing agent recorded in real time to a histogram in the sample distillation time, so that a detector can easily judge the conclusion whether the ammonia is completely distilled.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an analysis map for detecting the completion of ammonia distillation based on a full-automatic Kjeldahl apparatus color method provided in the embodiment of the invention;
FIG. 2 is an analytical map for detecting incomplete ammonia distillation based on a full-automatic Kjeldahl determination instrument color method provided in the embodiment of the invention;
FIG. 3 is a graph of the total amount of ammonia gas in the titration cup versus time;
FIG. 4 is a graph showing the amount of ammonia gas stored in the titration cup and the amount of ammonia gas added in the titration cup as a function of time.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for detecting complete ammonia distillation based on a full-automatic Kjeldahl determination instrument color method comprises the following steps: step S10: putting an organic compound sample containing protein, concentrated sulfuric acid and a catalyst into a test tube to be heated and digested together, so that the protein is decomposed, decomposed ammonia radical ions and sulfate radical ions are combined to generate ammonium sulfate, then dissociating ammonia gas under the action of alkaline distillation, cooling the dissociated ammonia gas and water vapor together through a condenser pipe to form ammonia water, and feeding the ammonia water into a titration cup filled with boric acid; step S20: dripping hydrochloric acid or sulfuric acid titration solution with known concentration into the titration cup, detecting the titration speed and recording in real time; step S30: before the distillation is finished, the titration speed is changed from high to low along with the neutralization of the ammonia gas by the standard acid, the interval time of slow dripping is gradually prolonged, or the titration is not carried out in unit time, and the ammonia gas is judged to be completely distilled. The titration speed can be measured by the pulse number of the stepping motor, the detected data is sent to the processor in real time, the processor receives and stores the real-time titration speed and processes the titration speed, the interval time of the slow drops gradually becomes longer before the distillation is finished, or no titration is carried out in a certain unit time, and the distillation is finished, the detection of the sample is finished, namely the ammonia gas is judged to be completely distilled, at the moment, the nitrogen content of the sample can be calculated according to the volume of the consumed standard liquid, so that whether the ammonia gas is completely distilled is judged by detecting the titration speed in real time, and the detection data of the Kjeldahl apparatus can be more accurate and stable and can be repeated; and the correctness of the calculated data of the sample is also made a basis.
The step S20 further includes a step S21: and (3) dripping hydrochloric acid or sulfuric acid titration solution with known concentration into the titration cup, displaying the pH value by the color developing agent, detecting the color change of the color developing agent and recording in real time.
The step S20 further includes a step S22: and (3) detecting that the color developing agent in the titration cup filled with the boric acid is red, changing the color developing agent into blue after ammonia enters the titration cup, changing the color developing agent into reddish when titration is carried out to be balanced, reducing the titration speed along with less ammonia entering the titration cup generated by the distilled sample, and slowly dripping at intervals of larger and larger until the distillation is finished, namely judging that the ammonia is completely distilled.
The color change of the color developing agent can be detected through the color sensor, the detected data are sent to the processor in real time, the processor receives and stores the real-time color change and processes the color change, the detected color is changed from red to blue, and finally the color change is reddish, the titration is finished, and the ammonia gas is judged to be completely distilled. The color developing agent can adopt bromocresol green and methyl red, and has acid color development red, alkaline color development blue and neutral color non-change; the ammonia gas distilled off was alkaline and thus blue in color.
The method for detecting the completion of ammonia distillation based on the full-automatic Kjeldahl apparatus color method further comprises the step S40: detecting the establishment of an analysis map of the complete ammonia distillation, setting the distillation time of a sample as an X axis, setting the titration amount as a Y axis, and extending a color frame from an original point along the X axis direction, wherein the color frame is used for representing the real-time color in the titration cup; drawing the titration speed recorded in real time into a histogram in the sample distillation time, wherein the histogram is drawn above a color frame; changes in color of the developer recorded in real time were added to the histogram and color box during the sample distillation time. An analysis map for detecting the completion of ammonia distillation is generated by modeling data stored in the processor and displayed by a display, so that detection personnel can conveniently check whether the ammonia distillation is complete in real time and check the consumption condition of the standard liquid and the nitrogen content change of the sample in real time.
Through the real-time detection of the change of the titration speed and the color of the color developing agent, the detection data of the Kjeldahl determination instrument can be more accurate and stable, the change of the color developing agent recorded in real time is added to the histogram in the sample distillation time, the combination of the color developing agent and the histogram can enable the established analysis map for detecting the complete ammonia gas distillation to be more visual, and a detector can easily judge the conclusion whether the ammonia gas is completely distilled.
As shown in figure 1, the analysis map is a real-time analysis map for detecting the complete ammonia distillation based on a full-automatic Kjeldahl apparatus:
the ordinate (Y-axis) is the titration amount, with the unit ul, higher representing a larger titration amount.
The abscissa (X-axis) is the distillation titration time in seconds.
A is a color frame: and displaying the real-time display color of the titration cup, wherein the color represents the pH value in the titration cup. Observing the color box, it is known whether the acid-base equilibrium point is reached by the distillation titration (the equilibrium point also appears during the distillation process).
B is rapid titration: indicating that a large amount of ammonia gas had entered the titration cup.
C is the titration interval, longer time represents lower titration frequency, indicating less ammonia gas production.
D is slow titration: at this time, the amount of the titration is small and the amount of the ammonia gas stored in the titration cup is small.
The color frame A is displayed with red color, titration is started at the beginning of distillation for 90 seconds, a large amount of ammonia gas is distilled to a titration cup at the moment, the highest titration speed is 150 ul/s, the color frame B is displayed with blue color, the titration speed automatically changes to 10 ul/s, 2 ul/s and 2ul/2 s along with the neutralization of the ammonia gas in the titration cup and the reduction of the distilled ammonia gas, gradually changing reddish color is displayed in the color frame D, and the titration end point is reached if the detected color changes from red to blue finally to reddish color, and the titration is finished. The titration speed is high, which indicates that a large amount of ammonia is neutralized by the standard acid, and then little ammonia is distilled out, and the titration speed is reduced along with the reduction of the ammonia; finally, the titration interval time is gradually lengthened, which shows that less and less ammonia gas is distilled, and the ammonia gas is almost completely distilled; namely, at the last stage of distillation titration, the titration amount is reduced, the slow titration frequency is reduced, and even if a small amount of titration is distilled later, the detection result is not influenced, which indicates that the ammonia gas is completely distilled.
If titration is carried out before the distillation is finished, the ammonia gas is still distilled out frequently, and as shown in figure 2, within a certain distillation time, the titration speed is still faster, new ammonia gas is generated, and it can be obviously seen that the ammonia gas in the sample is not completely distilled, so that the obtained consumption standard liquid volume and the data of the nitrogen content of the sample calculated from the consumption standard liquid volume are lower, the distillation time can be prolonged, and the data are more accurate and stable.
As shown in fig. 3, which is a graph of the total amount of ammonia in the titration cup with respect to time, when the distillation time is set to be less than t1, the ammonia is not completely distilled, and the data has errors, and if the distillation time is greater than t2, the detection of ammonia does not change significantly with t1, but the detection efficiency is reduced. It is reasonable to set the distillation time between t1 and t 2. As for selecting t1 or t2, the user selects according to the actual detection precision requirement, such as milk protein with low detection requirement, t1 can be selected, and such as Cordyceps with high detection requirement, t2 can be selected, so that the data is more accurate.
According to the detected titration speed, a relation graph of the ammonia gas storage in the titration cup during titration and the time can be drawn as shown in fig. 4, when the standard acid is titrated at a high speed, a large amount of ammonia gas in the titration cup is consumed, the corresponding titration speed is reduced along with the decrease of the ammonia gas, and the interval time of slow dropping is gradually increased. If the milk protein is not high in detection requirement, the subsequent extremely small amount of ammonia gas is not enough to influence the accuracy of the data, and the ammonia gas can be judged to be completely distilled in order to improve the detection efficiency; if the cordyceps sinensis is cordyceps sinensis with high detection requirement, the distillation time is prolonged until no titration is carried out within a certain time, namely, the ammonia gas is judged to be completely distilled, so that the data is more accurate, the relationship graph can help a detection user to determine that the distillation time provides scientific basis, meanwhile, the relationship graph also illustrates that the analysis graph for detecting whether the ammonia gas is completely distilled corresponds to the ammonia gas storage in the titration cup and the new increment relationship, and the scientificity of the analysis graph is explained in principle.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (4)
1. A method for detecting the completion of ammonia distillation based on a full-automatic Kjeldahl apparatus color method is characterized by comprising the following steps:
step S10: putting an organic compound sample containing protein, concentrated sulfuric acid and a catalyst into a test tube to be heated and digested together, so that the protein is decomposed, decomposed ammonia radical ions and sulfate radical ions are combined to generate ammonium sulfate, then dissociating ammonia gas under the action of alkaline distillation, cooling the dissociated ammonia gas and water vapor together through a condenser pipe to form ammonia water, and feeding the ammonia water into a titration cup filled with boric acid;
step S20: dripping hydrochloric acid or sulfuric acid titration solution with known concentration into the titration cup, detecting the titration speed and recording in real time;
step S30: before the distillation is finished, the titration speed is changed from high to low along with the neutralization of the ammonia gas by the standard acid, the interval time of slow dripping is gradually prolonged, or the titration is not carried out in unit time, and the ammonia gas is judged to be completely distilled.
2. The method according to claim 1, wherein step S20 further comprises step S21: and (3) dripping hydrochloric acid or sulfuric acid titration solution with known concentration into the titration cup, displaying the pH value by the color developing agent, detecting the color change of the color developing agent and recording in real time.
3. The method of claim 2, wherein the step S20 further comprises the step S22: the color developing agent in the titration cup filled with boric acid is detected to be red, the color developing agent is changed into blue after ammonia enters the titration cup, and the color developing agent is changed into reddish when the titration is started to be balanced;
and the titration speed is slowed down along with less and less ammonia entering the titration cup generated by distilling the sample, and slowly dropping with intervals of increasing and decreasing is carried out until the distillation is finished, namely the ammonia is judged to be completely distilled.
4. The method according to claim 3, further comprising step S40: detecting the establishment of an analysis map of the complete ammonia distillation, setting the distillation time of a sample as an X axis, setting the titration amount as a Y axis, and extending a color frame from an original point along the X axis direction, wherein the color frame is used for representing the real-time color in the titration cup;
drawing the titration speed recorded in real time into a histogram in the sample distillation time, wherein the histogram is drawn above a color frame;
changes in color of the developer recorded in real time were added to the histogram and color box during the sample distillation time.
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| 刘绍 等: "《全国应用型本科院校化学课程统编教材 食品分析与检验 第二版》", 31 August 2019 * |
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