CN103217501A - Method for determining carbon dioxide content in carbonated beverage - Google Patents

Method for determining carbon dioxide content in carbonated beverage Download PDF

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CN103217501A
CN103217501A CN2013101097476A CN201310109747A CN103217501A CN 103217501 A CN103217501 A CN 103217501A CN 2013101097476 A CN2013101097476 A CN 2013101097476A CN 201310109747 A CN201310109747 A CN 201310109747A CN 103217501 A CN103217501 A CN 103217501A
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sample
carbon dioxide
bottle
soda
dioxide content
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CN103217501B (en
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李海龙
刘梦茹
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The invention relates to a method for determining carbon dioxide content in carbonated beverage, and particularly relates to a method for quickly determining the carbon dioxide content in the carbonated beverage by headspace gas chromatography. The method comprises the following steps of: (1) preprocessing a sample; (2) establishing a standard curve; (3) performing sample detection through headspace-gas chromatography; (4) calculating the result. The method for determining carbon dioxide content in carbonated beverage has the beneficial effects of being capable of realizing batch detection, and having the advantages of being simple and convenient to operate, easy to master, high in detection sensitivity, accurate in determination result and high in interference rejection, and the like.

Description

A kind of method of measuring carbon dioxide content in the soda
Technical field
The present invention relates to a kind of CO 2 content determination method, is a kind of method of utilizing headspace gas chromatography to measure carbon dioxide content in the soda specifically, belongs to the food analysis detection range.
Background technology
Soda is one of modal drink in people's daily life, and it has unique salubrious taste and the irreplaceable function of quenching one's thirst of relieving summer heat.These character and the carbon dioxide of soda have confidential relation.When drinking soda, because increase in temperature makes carbon dioxide vaporization, produce excitement and also take away the human heat, institute is so that people produce a kind of refrigerant and eliminate the sensation of fatigue drinking the back.In addition, the carbon dioxide of capacity also can play sterilization, antibacterial effect in beverage.Yet, because carbon dioxide can not be higher than certain limiting the quantity of in blood of human body, so, if carbon dioxide content is excessive in the soda, can produce a kind of uncomfortable reaction of making us after drinking.The whether suitable product quality that is directly connected to of the content of carbon dioxide in the soda.Therefore, it is significant to controllable quality accurately to measure in the soda content of carbon dioxide.
The assay method of carbon dioxide mainly contains manometer method and titrimetry (comprising distillation titrimetry and potentiometric titration) etc. in the carbon current acid beverage, and these methods cut both ways.Wherein, the manometer method is easy and simple to handle, quick, but this precision of method is lower, easily produce error.And the titrimetry operation is more loaded down with trivial details and consuming time, brings very big inconvenience to mensuration.Therefore set up a kind of more easy, quick, accurately measure that the method for carbon dioxide content has realistic meaning in the soda.
Summary of the invention
The object of the present invention is to provide a kind of method of measuring carbon dioxide content in the soda, overcome the existing drawback of method of carbon dioxide content in the present analysis soda.Can realize batch detection according to this method, simple to operate and easy grasp, its analysis result accuracy height has certain practicality.Purpose of the present invention is achieved through the following technical solutions.
A kind of method of measuring carbon dioxide content in the soda comprises the steps:
(1) sample pretreatment: the soda of will not uncap is put into the refrigerating chamber of refrigerator, treats that bottle interior beverage opens bottle cap when freezing, adds the sufficient hydrogen aqueous solution of sodium oxide, immediately seals beverage bottle; Slowly rock after several minutes and put to room temperature, to be determined;
(2) set up typical curve: the capacity aqueous sulfuric acid that in a plurality of headspace sample bottles, adds equal volume respectively, and sealed sample bottle, in different sample bottles, add the different sodium carbonate standard water solution of measuring with injector successively then, again the headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, can obtain a typical curve between the amount of gained gas chromatography signal peak area and adding carbonate;
(3) sample detection: accurately measure an amount of pretreatment sample, be added to it in headspace sample bottle that seals and be equipped with sulfuric acid solution with injector, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, note the gas chromatography peak area of sample;
(4) result calculates: step (3) gained peak area and step (2) typical curve are compared, by calculating the content of carbon dioxide in the sample.
Further optimize, used sodium hydrate aqueous solution concentration is 6.0 ~ 12.0mol/L in the step (1), and addition amount of sodium hydroxide is 15 ~ 30mL/L, and treatment temperature is-5 ~ 0 ℃ in the refrigerating chamber, and the time is 45 ~ 120min.
Further optimize, the concentration of sodium carbonate standard water solution is 0.1 ~ 0.5mol/L described in the step (2); Aqueous sulfuric acid concentration is 1.0 ~ 2.0mol/L, and volume is 1.0 ~ 3.0mL.
Further optimize, the volume of the sodium carbonate standard water solution that adds described in the step (2) is 0.0 ~ 0.6mL.
Further optimize, the operating conditions of the head-space sampler described in step (2) and (3) is: 50 ~ 70 ℃ of injector furnace temps; Nitrogen gas pressure equilibration time 0.2 ~ 1.0 min in the head space bottle; Equilibration time 0.05 ~ 0.1 min of pipeline; Equilibration time 2.0 ~ the 4.0min of head space bottle in baking oven; Inflationtime 1.0 ~ the 3.0min of pipeline.
Further optimize, the operating conditions of the gas chromatography described in step (2) and (3) is: capillary column ID=0.53 mm, and length L=30 m(models are GS-Q, J ﹠W Scientific Inc., Folsom, CA); Column temperature is 35 ~ 75 ℃; Carrier gas is a high pure nitrogen, and its flow velocity is 3.0 ~ 3.5mL/min; Detecting device is thermal conductivity detector (TCD) (TCD), and detector temperature is 210 ~ 250 ℃.
Further optimize, sample volume is 0.5 ~ 2.0mL after the pre-service that is taken by weighing in the step (3).
Further optimize, the method for carbon dioxide content originally specifically may further comprise the steps in the described mensuration soda:
(1) sample pretreatment: the soda of will not uncap is put into the refrigerating chamber (5 ~ 0 ℃) of refrigerator, after placing 45 ~ 120min, treat that bottle interior beverage opens bottle cap when freezing, adding concentration rapidly is that (addition is 15 ~ 30mL/L) to 6.0 ~ 12.0mol/L sodium hydroxide solution, immediately seals beverage bottle.Slowly rock after several minutes and put to room temperature, to be determined.
(2) set up typical curve: in a series of headspace sample bottle, add the sulfuric acid that 1.0 ~ 3.0mL concentration is 1.0 ~ 2.0mol/L respectively, and sealed sample bottle, then with injector add 0.0,0.1,0.2,0.3,0.4,0.5 in the different sample bottles successively, 0.6mL concentration is the sodium carbonate standard solution of 0.1 ~ 0.5mol/L, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, can obtain a typical curve between the amount of gained gas chromatography signal peak area and adding carbonate.
(3) sample detection: accurately measure sample after the pre-service of 0.5 ~ 2.0mL, it is added to injector has sealed, and be equipped with in the headspace sample bottle of sulfuric acid solution, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, note the gas chromatography peak area of sample.
(4) result calculates: step (3) gained peak area and step (2) typical curve are compared, and by calculating the content of carbon dioxide in the sample, its computing formula is:
In the formula, m is the amount of carbonate in the sample that carries out head space-gas Chromatographic Determination that is obtained by typical curve; V 0For population of samples amasss; V 1For the sample volume that carries out head space-gas Chromatographic Determination; V 2For adding the volume of NaOH in the beverage bottle; 44 is the molecular weight of carbon dioxide; 60 is the molecular weight of carbonate.
Compared with prior art, advantage of the present invention and good effect are:
(1) grasp easy and simple to handle and easy;
(2) measure the process time weak point;
(3) reaction system is simple, has reduced error at measurment;
(4) antijamming capability is strong, and under the condition that is limited, the existence of other material in the sample can not impact mensuration;
(5) sensitivity of this method is higher.
Description of drawings
Fig. 1 is to be gas chromatography signal peak area and add the typical curve of corresponding relation between the amount of carbonate in the example.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.The present invention is not limited to following embodiment.Embodiment only is used to explain the present invention, and unrestricted the present invention all should belong to protection scope of the present invention for relating to simple change of the present invention.
Embodiment 1 measures the content of carbon dioxide in the soda
(1) sample pretreatment: the soda of will not uncap is put into the refrigerating chamber (4 ℃) of refrigerator, after placing 60min, treat that bottle interior beverage opens bottle cap when freezing, adding concentration rapidly is 12.0mol/L sodium hydroxide solution (addition is 25mL/L), immediately seals beverage bottle.Slowly rock after several minutes and put to room temperature, to be determined.
(2) set up typical curve: in a series of headspace sample bottle, add the sulfuric acid solution that 1.0mL concentration is 1.0mol/L respectively, and sealed sample bottle, then with injector add 0.0,0.1,0.2,0.3,0.4,0.5 in the different sample bottles successively, 0.6mL concentration is the sodium carbonate standard solution of 0.2mol/L, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, can obtain a typical curve between the amount of gained gas chromatography signal peak area and adding carbonate, as shown in Figure 1.
The operating conditions of described head-space sampler is: 50 ℃ of injector furnace temps; Nitrogen gas pressure equilibration time 0.2 min in the head space bottle; Equilibration time 0.05 min of pipeline; The equilibration time 2.0min of head space bottle in baking oven, degrees of shaking are strong level; The inflationtime 1.0min of pipeline.
The operating conditions of described gas chromatography is: capillary column ID=0.53 mm, and length L=30 m(models are GS-Q, J ﹠W Scientific Inc., Folsom, CA); Column temperature is 75 ℃; Carrier gas is a high pure nitrogen, and its flow velocity is 3.5mL/min; Detecting device is thermal conductivity detector (TCD) (TCD), and detector temperature is 250 ℃.
(3) sample detection: accurately measure sample after the pre-service of 1.0mL, it is added to injector has sealed, and be equipped with in the headspace sample bottle of sulfuric acid solution, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, note the gas chromatography peak area of sample.The operating conditions of head-space sampler and gas chromatography as hereinbefore.
(4) result calculates: step (3) gained peak area and step (2) typical curve are compared, and by calculating the content of carbon dioxide in the sample, its computing formula is:
In the formula, m is the amount of carbonate in the sample that carries out head space-gas Chromatographic Determination that is obtained by typical curve; V 0For population of samples amasss; V 1For the sample volume that carries out head space-gas Chromatographic Determination; V 2For adding the volume of NaOH in the beverage bottle; 44 is the molecular weight of carbon dioxide; 60 is the molecular weight of carbonate.
(5) measurement result is as shown in table 1.
Table 1
Embodiment 2 measures the content of carbon dioxide in the beer
(1) sample pretreatment: the beer of will not uncap is put into the refrigerating chamber (3 ℃) of refrigerator, after placing 60min, treat that bottle interior beverage opens bottle cap when freezing, adding concentration rapidly is 9.0mol/L sodium hydroxide solution (addition is 30mL/L), immediately seals beverage bottle.Slowly rock after several minutes and put to room temperature, to be determined.
(2) set up typical curve: in a series of headspace sample bottle, add the sulfuric acid solution that 1.0mL concentration is 1.0mol/L respectively, and sealed sample bottle, then with injector add 0.0,0.1,0.2,0.3,0.4,0.5 in the different sample bottles successively, 0.6mL concentration is the sodium carbonate standard solution of 0.2mol/L, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, can obtain a typical curve between the amount of gained gas chromatography signal peak area and adding carbonate, as shown in Figure 1.
The operating conditions of described head-space sampler is: 50 ℃ of injector furnace temps; Nitrogen gas pressure equilibration time 0.2 min in the head space bottle; Equilibration time 0.05 min of pipeline; The equilibration time 2.0min of head space bottle in baking oven, degrees of shaking are strong level; The inflationtime 1.0min of pipeline.
The operating conditions of described gas chromatography is: capillary column ID=0.53 mm, and length L=30 m(models are GS-Q, J ﹠W Scientific Inc., Folsom, CA); Column temperature is 75 ℃; Carrier gas is a high pure nitrogen, and its flow velocity is 3.5mL/min; Detecting device is thermal conductivity detector (TCD) (TCD), and detector temperature is 250 ℃.
(3) sample detection: accurately measure sample after the pre-service of 1.0mL, it is added to injector has sealed, and be equipped with in the headspace sample bottle of sulfuric acid solution, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, note the gas chromatography peak area of sample.The operating conditions of head-space sampler and gas chromatography as hereinbefore.
(4) result calculates: step (3) gained peak area and step (2) typical curve are compared, and by calculating the content of carbon dioxide in the sample, its computing formula is:
In the formula, m is the amount of carbonate in the sample that carries out head space-gas Chromatographic Determination that is obtained by typical curve; V 0For population of samples amasss; V 1For the sample volume that carries out head space-gas Chromatographic Determination; V 2For adding the volume of NaOH in the beverage bottle; 44 is the molecular weight of carbon dioxide; 60 is the molecular weight of carbonate.
(5) measurement result is as shown in table 2.
Table 2
By above-mentioned example and result as can be known, can realize batch detection according to method provided by the invention, simple to operate and easy grasp, its testing result accuracy height has certain practicality.

Claims (8)

1. a method of measuring carbon dioxide content in the soda is characterized in that, comprises the steps:
(1) sample pretreatment: the soda of will not uncap is put into the refrigerating chamber of refrigerator, treats that bottle interior beverage opens bottle cap when freezing, adds the sufficient hydrogen aqueous solution of sodium oxide, immediately seals beverage bottle; Slowly rock after several minutes and put to room temperature, to be determined;
(2) set up typical curve: the capacity aqueous sulfuric acid that in a plurality of headspace sample bottles, adds equal volume respectively, and sealed sample bottle, in different sample bottles, add the different sodium carbonate standard water solution of measuring with injector successively then, again the headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, can obtain a typical curve between the amount of gained gas chromatography signal peak area and adding carbonate;
(3) sample detection: accurately measure an amount of pretreatment sample, be added to it in headspace sample bottle that seals and be equipped with sulfuric acid solution with injector, ready headspace sample bottle is positioned on the sample stage, carry out head space-gas chromatographic detection then, note the gas chromatography peak area of sample;
(4) result calculates: step (3) gained peak area and step (2) typical curve are compared, by calculating the content of carbon dioxide in the sample.
2. the method for carbon dioxide content in the mensuration soda according to claim 1, it is characterized in that: used sodium hydrate aqueous solution concentration is 6.0 ~ 12.0mol/L in the step (1), addition amount of sodium hydroxide is 15 ~ 30mL/L, treatment temperature is-5 ~ 0 ℃ in the refrigerating chamber, and the time is 45 ~ 120min.
3. the method for carbon dioxide content in the mensuration soda according to claim 1 is characterized in that: the concentration of sodium carbonate standard water solution is 0.1 ~ 0.5mol/L described in the step (2); Aqueous sulfuric acid concentration is 1.0 ~ 2.0mol/L, and volume is 1.0 ~ 3.0mL.
4. the method for carbon dioxide content in the mensuration soda according to claim 1 is characterized in that: the volume of the sodium carbonate standard water solution that adds described in the step (2) is 0.0 ~ 0.6mL.
5. the method for carbon dioxide content in the mensuration soda according to claim 1 is characterized in that: the operating conditions of the head-space sampler described in step (2) and (3) is: 50 ~ 70 ℃ of injector furnace temps; Nitrogen gas pressure equilibration time 0.2 ~ 1.0 min in the head space bottle; Equilibration time 0.05 ~ 0.1 min of pipeline; Equilibration time 2.0 ~ the 4.0min of head space bottle in baking oven; Inflationtime 1.0 ~ the 3.0min of pipeline.
6. the method for carbon dioxide content in the mensuration soda according to claim 1 is characterized in that: the operating conditions of the gas chromatography described in step (2) and (3) is: capillary column ID=0.53 mm, length L=30 m; Column temperature is 35 ~ 75 ℃; Carrier gas is a high pure nitrogen, and its flow velocity is 3.0 ~ 3.5mL/min; Detecting device is thermal conductivity detector (TCD) (TCD), and detector temperature is 210 ~ 250 ℃.
7. the method for carbon dioxide content in the mensuration soda according to claim 1 is characterized in that: sample volume is 0.5 ~ 2.0mL after the pre-service that is taken by weighing in the step (3).
8. the method for carbon dioxide content in the mensuration soda according to claim 1 is characterized in that: calculating the formula that adopts described in the step (4) is:
In the formula, m is the amount of carbonate in the sample that carries out head space-gas Chromatographic Determination that is obtained by typical curve; V 0 For population of samples amasss; V 1For the sample volume that carries out head space-gas Chromatographic Determination; V 2 For adding the volume of NaOH in the beverage bottle; 44 is the molecular weight of carbon dioxide; 60 is the molecular weight of carbonate.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103698437A (en) * 2014-01-13 2014-04-02 福建农林大学 Method for quickly detecting starch coated amount in modified calcium carbonate filler through headspace gas chromatography
CN103868840A (en) * 2014-03-26 2014-06-18 南京中医药大学 Determination method of molecular weight cutoff of ultrafiltration membrane
CN106442860A (en) * 2016-08-31 2017-02-22 山东新华制药股份有限公司 Measuring method of carbonate content in sevelamer carbonate
CN107589201A (en) * 2017-09-18 2018-01-16 华南理工大学 A kind of method for reacting headspace gas chromatography measure amino acid content

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN102507762A (en) * 2011-10-18 2012-06-20 哈尔滨工程大学 Gas chromatography detection method for free carbon dioxide, carbonate and bicarbonate in water

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CN102507762A (en) * 2011-10-18 2012-06-20 哈尔滨工程大学 Gas chromatography detection method for free carbon dioxide, carbonate and bicarbonate in water

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Title
马茜: "化学转化顶空气相色谱法测定煤中碳酸盐二氧化碳", 《分析化学(FENXI HUAXUE)研究简报》, vol. 29, no. 10, 31 October 2001 (2001-10-31), pages 1202 - 1204 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103698437A (en) * 2014-01-13 2014-04-02 福建农林大学 Method for quickly detecting starch coated amount in modified calcium carbonate filler through headspace gas chromatography
CN103868840A (en) * 2014-03-26 2014-06-18 南京中医药大学 Determination method of molecular weight cutoff of ultrafiltration membrane
CN106442860A (en) * 2016-08-31 2017-02-22 山东新华制药股份有限公司 Measuring method of carbonate content in sevelamer carbonate
CN107589201A (en) * 2017-09-18 2018-01-16 华南理工大学 A kind of method for reacting headspace gas chromatography measure amino acid content

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