CN108037215B - Detection method for measuring ammonia content in tipping paper water-based ink by using ion chromatography - Google Patents
Detection method for measuring ammonia content in tipping paper water-based ink by using ion chromatography Download PDFInfo
- Publication number
- CN108037215B CN108037215B CN201810017614.9A CN201810017614A CN108037215B CN 108037215 B CN108037215 B CN 108037215B CN 201810017614 A CN201810017614 A CN 201810017614A CN 108037215 B CN108037215 B CN 108037215B
- Authority
- CN
- China
- Prior art keywords
- solution
- water
- sample
- based ink
- ammonia content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000001514 detection method Methods 0.000 title claims abstract description 18
- 238000004255 ion exchange chromatography Methods 0.000 title claims abstract description 15
- 239000000523 sample Substances 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 29
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000012498 ultrapure water Substances 0.000 claims abstract description 13
- 238000010790 dilution Methods 0.000 claims abstract description 12
- 239000012895 dilution Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000012488 sample solution Substances 0.000 claims abstract description 12
- 238000002470 solid-phase micro-extraction Methods 0.000 claims abstract description 10
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 229940098779 methanesulfonic acid Drugs 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 150000002500 ions Chemical class 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 13
- 239000012086 standard solution Substances 0.000 claims description 9
- 239000003480 eluent Substances 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- -1 Dionex ion Chemical class 0.000 claims description 2
- 239000012224 working solution Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 48
- 235000019504 cigarettes Nutrition 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 239000000654 additive Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000010812 external standard method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
Images
Classifications
-
- 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
- G01N30/02—Column chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a method for detecting ammonia content in tipping paper water-based ink by using ion chromatography. In particular to a weighing M1g water-based ink sample added to v1Extracting with mL acid solution, taking out the container, placing the container until the supernatant is clear, and taking out the container2Clarifying the supernatant of mL, filtering the aqueous gloss oil with an ultrafiltration membrane, and filtering with M2g, cleaning the filter membrane by ultrapure water, collecting the filtrate and the cleaning solution, transferring 5mL of the filtrate and the cleaning solution, and pressurizing to pass through C18And (3) leaching the solid-phase microextraction column by using 15.0mL of methane sulfonic acid or sulfuric acid solution with the concentration of 0.005-0.01 mol/L for several times, collecting filtrate and washing liquid to obtain a sample solution to be detected, analyzing and detecting by using an ion chromatograph, calculating the ammonia content C of the sample solution to be detected by using a standard curve, and finally multiplying by a corresponding dilution multiple to obtain the final ammonia content. The invention has the advantages of rapid and convenient detection process, accurate detection content result and high sensitivity.
Description
Technical Field
The invention relates to an ion chromatography detection method for separating micromolecule components and macromolecular substances of water-soluble ink used for cigarette tipping paper and quantitatively analyzing ammonia content of the micromolecule components and the macromolecular substances.
Background
The quality of the tipping paper for cigarettes directly influences the experience of consumers, so that the tipping paper for cigarettes is gradually valued. In recent years, due to the enhancement of health consciousness of people, the production technology of cigarette tipping paper has been greatly improved, such as printing by using alcohol-soluble ink instead of ester-soluble ink, punching holes on the tipping paper to dilute harmful components in mainstream smoke, and the like.
As with other printing inks, the aqueous ink comprises colorants, binders, solvents, and adjuvants as the primary components. Only by adjusting the proportion of the components of the printing ink, the due printability and the service performance of the printing ink can be achieved, and the printing ink can be well matched with a printing plate, a printing machine and a printing material, so that the printing process can be smoothly carried out.
The auxiliary agent, also called additive, is an auxiliary component of the ink, and is used to adjust the printability of the ink, and for various purposes, various kinds and amounts of the auxiliary agent are added to the preparation of the ink to adjust the fluidity, drying property, color tone, and the like of the ink. The physical and chemical properties of the aqueous ink are largely determined by the additives in the aqueous ink. The addition of additives to aqueous inks to achieve certain specified physical and chemical properties is a common practice in the flexographic printing industry. In the aqueous ink, the coloring material, resin and solvent account for about 95% of the ink components, and the remaining 5% are various additives. The lubricant comprises (1) a lubricant, (2) a surfactant, (3) a cross-linking agent, (4) an adhesion promoter, (5) a defoaming agent, (6) a bactericide, (7) a mineral substance, (8) an oxidizing agent and (9) a plasticizer. The mineral substance in the water-based ink is usually ammonia water, and can dissolve the resin binder, maintain the stable pH value of the water-based ink and ensure the printability of the water-based ink. Later researches find that the chemical property of ammonia is unstable and has pungent smell, so that part of water-based ink is replaced by amine compounds, and the stability of the ammonia is better, but the ammonia also has the potential of negative influence on the cigarette sense.
Most central cigarette products in the tobacco industry are too cigarette products, and the requirements on the cigarette sensory quality are very strict. However, the cigarette industry tipping paper production department usually uses national standards YC 263-.
Moreover, water-based inks contain water and cannot be directly injected into a gas chromatograph in general; the high molecular resin has high viscosity and boiling point, contains some impurities which are difficult to volatilize, is not suitable for direct sample injection chromatographic analysis, can pollute parts of instruments, and can not finish accurate quantitative analysis of ammonia by headspace equipment. The conventional detection method does not relate to the detection of ammonia in the water-based ink by ion chromatography with the assistance of a pretreatment technology.
Disclosure of Invention
The invention aims to provide a method for detecting the ammonia content in tipping paper water-based ink by using ion chromatography, which utilizes a molecular filter membrane to selectively separate small molecules and macromolecular components; the small molecular components can be directly injected into various chromatographs, including ion chromatograph detection. The quantitative analysis by an external standard method does not cause the pollution of instrument parts, and the specific content of the ammonia is quantitatively detected by using ion chromatography.
Aiming at the technical scheme that the prior art is insufficient, the invention provides the following technical scheme that: a detection method for measuring the ammonia content in tipping paper water-based ink by using ion chromatography is characterized by comprising the following specific steps:
(1) accurate weighing M1g aqueous ink sample, placing in a container, adding it v1Placing the mL acid solution in an oscillator, oscillating at the rotating speed of 160-200R/min for 5-8 minutes, extracting, taking out the container, and placing the container until the upper layer solution is clear; wherein the mass M of the aqueous ink sample15-20 g of acid solution is added15-10 mL;
(2) accurately taking out the supernatant in the step (1)2mL, the aqueous ink was filtered through an ultrafiltration membrane at an operating pressure of 1.5 × 105Pa～3.0×105Pa, the average pore diameter of the selected membrane is 0.1-0.4 μm; after filtration, with M2g, cleaning the filter membrane by using ultrapure water, and collecting and combining the filtrate and the cleaning solution to obtain a water-based ink solution; mass M of water-based ink sample1And mass M of ultrapure water2The following relationship is satisfied: m1<M2<10M1(ii) a The amount v of supernatant in the taking step (1)25.0-10.0 mL, and the dilution factor by filtration is (M)1+M2)v1/M1v2；
(3) Accurately transferring 5.0mL of the filtered water-based ink solution, and pressurizing to pass through C18Keeping the flow rate of the solid-phase microextraction column at 0.5-2 mL/min, eluting the column with 15.0mL of methanesulfonic acid or sulfuric acid solution with the concentration of 0.005-0.01 mol/L for several times, collecting filtrate and washing liquid, and uniformly mixing to obtain a sample solution to be detected, wherein the eluent C is18The dilution factor caused by the solid phase micro-extraction column is 4 times;
(4) preparing standard working solutions of ammonia with different concentrations by using a sulfuric acid solution with the concentration of 0.005mol/L, analyzing the standard solutions by using ion chromatography, and drawing a standard curve of a component to be detected, wherein one coordinate of the standard curve is the concentration of a standard substance of the component to be detected, and the other coordinate of the standard curve is the peak area of a corresponding peak of the standard substance of the component to be detected;
(5) analyzing and detecting the sample solution to be detected in the step (3) by using an ion chromatograph to obtain a related chromatogram, and calculating NH+ 4Then calculating the ammonia content C of the sample solution to be measured according to the standard curve obtained in the step (4), and multiplying the ammonia content C by the ammonia content C18The dilution factor by solid phase microextraction column was 4 times and the dilution factor by filtration was (M)1+M2)v1/M1v2Calculating the total ammonia amount M in the water-based ink sample, wherein the calculation formula is as follows:
M＝4Cv1·(M1+M2)/(v2·M1) (1)
wherein M represents the total ammonia content, mg/L; c-measured value of ammonia content, mg/L; m1-water based ink sample mass, g; m2-mass of ultrapure water used for cleaning the filtration membrane, g; v. of1-volume of extracted acid, mL; v. of2Removing the volume of the extract liquid, mL;
the ion chromatographic column adopts Dionex IonPacTMA CS19 or CS12A chromatographic column with the diameter of 4mm × 250mm, eluent which is methane sulfonic acid solution, the flow rate of 1.0mL/min, the sample injection amount of 10-30 mu L, the column temperature of 30-40 ℃ and the detector pool temperature of 35-50 ℃.
The invention has the following excellent technical scheme: the acid solution in the step (1) is methane sulfonic acid or sulfuric acid with the mass concentration of 0.005-0.02 mol/L.
The invention has the following excellent technical scheme: the standard solutions prepared in the step (4) are respectively as follows: 0.01mg/L, 0.05mg/L, 0.2mg/L, 0.6mg/L, 2.0mg/L of a penta-ammonia standard solution.
The standard ammonia liquid and the ammonia standard solution in the invention; acid liquor: methane sulfonic acid, sulfuric acid solution; filter membrane leacheate: ultrapure water.
The method utilizes an ultrafiltration membrane to selectively separate low molecular weight impurity components (including ammonia, ethanol, acetone and the like) and macromolecular components (including soluble resin and the like) of the water-based ink; and purifying by a C18 solid phase microextraction column, and intensively collecting ammonia components related to sensory quality, so that ion chromatographic analysis becomes a feasible method, and the accuracy of subsequent detection is improved. For target ammonia which cannot be detected and cannot be accurately detected by directly using a headspace series GC-MS instrument and a gas phase hydrogen flame ionization detector (GC-FID), the method can complete detection work; the ammonia content can be detected by a separation technology and by directly feeding a sample into the ion chromatography.
The method separates the volatile components of the water-based ink sample by the ultrafiltration membrane, eliminates the interference of macromolecular substances, can detect some components which cannot be accurately detected by the conventional method, reduces detection errors, eliminates the interference of substances with higher viscosity and larger molecular weight, can directly sample ion chromatographic analysis, has low requirements on a temperature rise program and a chromatographic column, is quick and convenient in detection process, and has accurate detection content result and high sensitivity.
Drawings
Fig. 1 is a standard graph in the example.
Detailed description of the invention
In order that the invention may be further understood, preferred embodiments of the invention are described below with reference to the following examples.
In the invention, a small amount of sulfuric acid or methanesulfonic acid is added as an extraction liquid, and volatile components and components with higher boiling points are separated by an ultrafiltration membrane; the dosage of the solvent is small, so that the effect of separating and enriching target analytes is achieved; and detecting the content of the volatile components by directly injecting an ion chromatograph through an external standard method. The solvent in the invention can meet the basic requirement of direct sample injection ion chromatograph; the solvent is a low boiling point substance which does not exist in the sample to be detected; the solubility of the solvent and the measured component is good, but the polarity difference cannot be too similar, so that the chromatographic peak of the solvent and the chromatographic peak of the measured component can be completely separated; the solvent is not chemically reactive with the component to be tested. The solvent is therefore preferably ultrapure water or an acid solution.
The preferred embodiment of the invention is as follows:
example 1, for the detection of ammonia content in aqueous ink of four different cigarette tipping papers, the specific process is as follows:
(1) sample pretreatment and purification: m is accurately weighed by the pin1g four aqueous ink samples, placing in a ground conical flask, adding v1After the dissolved and sealed cover of the methane sulfonic acid with the concentration of 0.01mol/L, the mixture is placed in an oscillator to be oscillated for 6 minutes at the rotating speed of 160R/min; taking out the conical flask, placing the conical flask into an upper layer liquid, clarifying and collecting upper layer clarified liquid of the four water-based ink samples; wherein, the mass M of the four water-based ink samples1Amount v of acid solution1See table 1, respectively;
(2) accurately taking out the supernatant liquid of the four water-based ink samples in the step (1) respectively2mL, filtering the aqueous ink with an ultrafiltration membrane at an operating pressure of 2 × 105Pa, the average pore diameter of the selected membrane is 0.3 mu m; after filtration, with M2g, cleaning the filter membrane by using ultrapure water, and collecting and combining the filtrate and the cleaning solution to obtain four aqueous ink sample solutions; mass M of water-based ink sample1And mass M of ultrapure water2The following relationship is satisfied: 0.5M1<M2<5M1(ii) a The dilution factor resulting from the filtration is (M)1+M2)v1/M1v2(ii) a Mass M of cleaning solvent for the four aqueous ink samples2And the amount v of supernatant2See table 1, respectively;
TABLE 1 weighing the sample parameters and the dilution ratio
| Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 | |
| Water-based ink M1(g) | 9.431 | 5.996 | 2.154 | 9.882 |
| Ultrapure water M2(g) | 10.157 | 30.004 | 20.014 | 40.133 |
| V1(mL) | 5.0 | 20.0 | 10.0 | 10.0 |
| V2(mL) | 5.0 | 10.0 | 8.0 | 5.0 |
| 4v1·(M1+M2)/(v2·M1) | 8.308 | 48.032 | 51.458 | 40.490 |
(3) Precisely transferring 5mL of the four aqueous ink sample solutions obtained in the step (2), and pressurizing the solution to C18The solid phase micro-extraction column keeps the flow rate at 1-5 mL/min; eluting with 15.0mL methanesulfonic acid with concentration of 0.01mol/L for several times, collecting filtrate and washing liquid, mixing uniformly to obtain sample solution to be tested, wherein the eluent C is18The dilution factor caused by the solid phase micro-extraction column is 4 times;
(4) the ion chromatographic column adopts Dionex IonPacTMA CS19 or CS12A chromatographic column with the diameter of 4mm and the diameter of × 250mm, leacheate which is methane sulfonic acid solution, the flow rate is 2.0mL/min, the sample amount is 20 mu L, the column temperature is 35 ℃, the detector pool temperature is 45 ℃,
gradient conditions:
gradient elution procedure for leacheate
(5) Drawing a standard curve: performing fixed dissolution by using 0.005mol/L sulfuric acid solution, wherein the concentration of a standard curve is 0.011, 0.049, 0.205, 0.597 and 2.034mg/L, respectively analyzing the five-grade standard solution in an ion chromatograph according to the ion chromatography conditions in the step (4) to obtain a corresponding standard curve of each measured component, and as shown in figure 1, the form of a linear fitting equation is Y ═ aX + b; one coordinate of the standard curve is the concentration of a standard substance of the component to be detected, and the other coordinate is the peak area of a peak corresponding to the standard substance of the component to be detected; the standard curve equation is drawn by ion chromatography of one to five standard solutions of each target substance and is shown in table 2.
TABLE 2 Standard Curve equation obtained by GC-MS analysis of each component to be measured
| Target object | Standard curve | Relative deviation R |
| Ammonia | Y＝0.488X+0.152 | 0.99995 |
Remarking: x is the peak area of the corresponding peak of the target; y is target concentration (mg/L)
(6) Analyzing and detecting the sample solution to be detected in the step (3) by using an ion chromatograph under the ion chromatographic conditions as in the step (4), obtaining a related chromatogram, and calculating NH+ 4Then calculating the ammonia content C in the solution of the sample to be detected according to the standard curve obtained in the step (5), and calculating the total ammonia amount M in each aqueous gloss oil sample according to the following calculation formula:
M＝4Cv1·(M1+M2)/(v2·M1) (1)
wherein M represents the total ammonia content, mg/L; c-measured value of ammonia content, mg/L; m1-water based ink sample mass, g; m2-mass of ultrapure water used for cleaning the filtration membrane, g; v. of1-volume of extracted acid, mL; v. of2Removing the volume of the extract liquid, mL;
the ammonia content of the sample obtained by the detection and analysis of the ion chromatograph is shown in table 3,
TABLE 3 Ammonia detection results
By the technical method provided by the invention, the ammonia content in the four samples is detected, and whether the product of a supplier is qualified or not is judged according to the ammonia content. For example, sample nos. 1 and 2 had low ammonia content, so the standard passed; and the sample 4 with too high ammonia content exceeds the internal control standard limit, and is judged to be unqualified. The invention provides important guarantee for improving the quality of the tipping paper product.
Claims (2)
1. A detection method for measuring the ammonia content in tipping paper water-based ink by using ion chromatography is characterized by comprising the following specific steps:
(1) accurate weighing M1g aqueous ink sample, placing in a container, adding it v1Placing the mL acid solution in an oscillator, oscillating at the rotating speed of 160-200R/min for 5-8 minutes, extracting, taking out the container, and placing the container until the upper layer solution is clear; wherein the mass M of the aqueous ink sample15-20 g of acid solution is added15-10 mL; the acid solution is methane sulfonic acid or sulfuric acid with the mass concentration of 0.005-0.02 mol/L;
(2) accurately taking out the supernatant in the step (1)2mL, the aqueous ink was filtered through an ultrafiltration membrane at an operating pressure of 1.5 × 105Pa～3.0×105Pa, the average pore diameter of the selected membrane is 0.1-0.4 μm; after filtration, with M2g, cleaning the filter membrane by using ultrapure water, and collecting and combining the filtrate and the cleaning solution to obtain a water-based ink solution; mass M of water-based ink sample1And mass M of ultrapure water2The following relationship is satisfied: m1<M2<10M1(ii) a The amount v of supernatant in the taking step (1)25.0-10.0 mL, and the dilution factor by filtration is (M)1+M2)v1/M1v2；
(3) Accurately transferring 5.0mL of the filtered water-based ink solution, and pressurizing to pass through C18Keeping the flow rate of the solid-phase microextraction column at 0.5-2 mL/min, eluting the column with 15.0mL of methanesulfonic acid or sulfuric acid solution with the concentration of 0.005-0.01 mol/L for several times, collecting filtrate and washing liquid, and uniformly mixing to obtain a sample solution to be detected, wherein the eluent C is18The dilution factor caused by the solid phase micro-extraction column is 4 times;
(4) preparing standard working solutions of ammonia with different concentrations by using a sulfuric acid solution with the concentration of 0.005mol/L, analyzing the standard solutions by using ion chromatography, and drawing a standard curve of a component to be detected, wherein one coordinate of the standard curve is the concentration of a standard substance of the component to be detected, and the other coordinate of the standard curve is the peak area of a corresponding peak of the standard substance of the component to be detected;
(5) analyzing and detecting the sample solution to be detected in the step (3) by using an ion chromatograph to obtain a related chromatogram, and calculating NH+ 4Then calculating the ammonia content C of the sample solution to be measured according to the standard curve obtained in the step (4), and multiplying the ammonia content C by the ammonia content C18The dilution factor by solid phase microextraction column was 4 times and the dilution factor by filtration was (M)1+M2)v1/M1v2Calculating the total ammonia amount M in the water-based ink sample, wherein the calculation formula is as follows:
M=4Cv1·(M1+M2)/(v2·M1) (1)
wherein M represents the total ammonia content, mg/L; c-measured value of ammonia content, mg/L; m1-water based ink sample mass, g; m2-mass of ultrapure water used for cleaning the filtration membrane, g; v. of1-volume of extracted acid, mL; v. of2Removing the volume of the extract liquid, mL;
the ion chromatographic column adopts a Dionex ion Pac-shaped CS19 or CS12A chromatographic column, and the size of the chromatographic column is 4mm multiplied by 250 mm; leacheate: a methanesulfonic acid solution; flow rate: 1.0 mL/min; sample introduction amount: 10-30 mu L; column temperature: 30-40 ℃; detector pool temperature: 35-50 ℃.
2. The method for detecting the ammonia content in the tipping paper water-based ink by using ion chromatography according to claim 1, is characterized in that: the standard solutions prepared in the step (4) are respectively as follows: 0.01mg/L, 0.05mg/L, 0.2mg/L, 0.6mg/L, 2.0mg/L of a penta-ammonia standard solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810017614.9A CN108037215B (en) | 2018-01-09 | 2018-01-09 | Detection method for measuring ammonia content in tipping paper water-based ink by using ion chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810017614.9A CN108037215B (en) | 2018-01-09 | 2018-01-09 | Detection method for measuring ammonia content in tipping paper water-based ink by using ion chromatography |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108037215A CN108037215A (en) | 2018-05-15 |
| CN108037215B true CN108037215B (en) | 2020-09-08 |
Family
ID=62099428
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810017614.9A Active CN108037215B (en) | 2018-01-09 | 2018-01-09 | Detection method for measuring ammonia content in tipping paper water-based ink by using ion chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108037215B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110006892A (en) * | 2019-05-21 | 2019-07-12 | 上海烟草集团有限责任公司 | It is a kind of for water-based ink printing paper wrapper in ammonia content measuring method |
| CN112326856B (en) * | 2020-12-01 | 2022-10-04 | 上海烟草集团有限责任公司 | Method for rapidly detecting content of isothiazolinone compounds in water-based gloss oil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102331462A (en) * | 2011-06-22 | 2012-01-25 | 红云红河烟草(集团)有限责任公司 | Method for measuring ammonia content in water base adhesive for tobaccos |
| CN102590383A (en) * | 2012-02-13 | 2012-07-18 | 河北中烟工业有限责任公司 | Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously |
| CN104820035A (en) * | 2015-05-12 | 2015-08-05 | 川渝中烟工业有限责任公司 | Method for determining ammonia content in cigarette main stream smoke by ion chromatography |
| CN106908564A (en) * | 2017-02-28 | 2017-06-30 | 云南省烟草质量监督检测站 | Lithium, sodium, ammonia, potassium, magnesium, the method for calcium content in smoke-free tobacco product are determined simultaneously |
-
2018
- 2018-01-09 CN CN201810017614.9A patent/CN108037215B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102331462A (en) * | 2011-06-22 | 2012-01-25 | 红云红河烟草(集团)有限责任公司 | Method for measuring ammonia content in water base adhesive for tobaccos |
| CN102590383A (en) * | 2012-02-13 | 2012-07-18 | 河北中烟工业有限责任公司 | Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously |
| CN104820035A (en) * | 2015-05-12 | 2015-08-05 | 川渝中烟工业有限责任公司 | Method for determining ammonia content in cigarette main stream smoke by ion chromatography |
| CN106908564A (en) * | 2017-02-28 | 2017-06-30 | 云南省烟草质量监督检测站 | Lithium, sodium, ammonia, potassium, magnesium, the method for calcium content in smoke-free tobacco product are determined simultaneously |
Non-Patent Citations (4)
| Title |
|---|
| Method for the determination of ammonium in cigarette tobacco using ion chromatography;Christina Vaughan Watson 等;《REGULATORY TOXICOLOGY AND PHARMACOLOGY》;20150731;第72卷(第2期);第266-270页 * |
| 离子色谱法检测玉米中钾钠镁钙铵的方法研究;董瑞 等;《营养学报》;20071231;第29卷(第3期);第300-301页 * |
| 离子色谱法测定卷烟主流烟气中氨含量的方法改进;施文庄 等;《烟草科技》;20121231(第10期);第41-45页 * |
| 香烟中氨含量的优化离子色谱测定法;李伟青 等;《食品工业》;20151231;第36卷(第6期);第276-278页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108037215A (en) | 2018-05-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104597160B (en) | HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata | |
| CN104483427A (en) | Method for separating, enriching and detecting 12 antibiotics in drinking water source | |
| CN108037215B (en) | Detection method for measuring ammonia content in tipping paper water-based ink by using ion chromatography | |
| CN107091892A (en) | The method that the content of synthetic coloring matter in food is tested using high performance liquid chromatography | |
| CN112526007B (en) | Method for separating and detecting contents of m-cresol and p-cresol by using ultra-high liquid chromatography and application | |
| CN105372371B (en) | Ion chromatographic method and the application of reconstituted tobacco oxalate, amber acid radical, sulfate radical and phosphate radical are determined simultaneously | |
| CN101354349A (en) | Method for measuring protein nitrogen content in tobacco | |
| CN103115994B (en) | Method for rapidly measuring Cr(III) and Cr(VI) ion in tipping paper for cigarette | |
| CN109655557A (en) | A kind of detection method of Bu Waxitan and its impurity | |
| CN112326855A (en) | Method for rapidly measuring 12 water extracts of tea | |
| CN108152425B (en) | Method for detecting lignanoids in sesame oil by high performance liquid chromatography | |
| CN107315058A (en) | A kind of method of total ginkgoic acid in detection ginkgo biloba succi | |
| CN111413432B (en) | Method for detecting trace PFOA (perfluorooctanoic acid) in fluorine-containing polymer emulsion product | |
| CN105334283B (en) | Simultaneous Determination reconstituted tobacco oxalate, amber acid radical, the sample-pretreating method of sulfate radical and phosphate radical | |
| CN108181393B (en) | Method for detecting hydroxyethyl hexahydro-s-triazine in plastic product | |
| CN108195966B (en) | Method for detecting ammonia content in aqueous gloss oil of cigarette tipping paper | |
| CN107941965A (en) | A kind of cigarette tipping paper water-based gloss oil volatile ingredient detection method | |
| CN108896698A (en) | Ion chromatographic method and application a kind of while that measure sorb acid group in reconstituted tobacco, phosphate radical and citrate | |
| CN108195958B (en) | Method for detecting N, N-diglycidyl-4-glycidyloxyaniline in plastic product | |
| CN107991402B (en) | Method for simultaneously detecting 6 groups of azo sulfonic pigment isomers in bean products | |
| CN111175393A (en) | Method for detecting laurolactam in oil food simulant by solid phase extraction-liquid chromatography | |
| CN106596766A (en) | Analysis method for content of macamide B in maca supercritical CO2 extract | |
| CN112345661B (en) | Method for determining content of florfenicol in veterinary drug gardenia flaviviridae oral liquid | |
| CN110057930A (en) | A kind of high-flux detection method of fresh milk multiple groups class residue of veterinary drug | |
| CN109709252B (en) | Detection method of epoxy polymer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |