CN108037215A - The detection method of ammonia content in a kind of tipping paper water-based ink using ion chromatography - Google Patents
The detection method of ammonia content in a kind of tipping paper water-based ink using ion chromatography Download PDFInfo
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- CN108037215A CN108037215A CN201810017614.9A CN201810017614A CN108037215A CN 108037215 A CN108037215 A CN 108037215A CN 201810017614 A CN201810017614 A CN 201810017614A CN 108037215 A CN108037215 A CN 108037215A
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- ammonia content
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 80
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 43
- 238000001514 detection method Methods 0.000 title claims abstract description 25
- 238000004255 ion exchange chromatography Methods 0.000 title claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 239000012488 sample solution Substances 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 12
- 239000012498 ultrapure water Substances 0.000 claims abstract description 12
- 238000002470 solid-phase micro-extraction Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 239000006210 lotion Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000004458 analytical method Methods 0.000 claims abstract description 4
- 238000005352 clarification Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 31
- 239000000523 sample Substances 0.000 claims description 28
- 150000002500 ions Chemical class 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 7
- UTEFBSAVJNEPTR-RGEXLXHISA-N loprazolam Chemical compound C1CN(C)CCN1\C=C/1C(=O)N2C3=CC=C([N+]([O-])=O)C=C3C(C=3C(=CC=CC=3)Cl)=NCC2=N\1 UTEFBSAVJNEPTR-RGEXLXHISA-N 0.000 claims description 6
- 229960003019 loprazolam Drugs 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- 239000012925 reference material Substances 0.000 claims description 5
- 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 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000012224 working solution Substances 0.000 claims description 2
- 239000002387 analytical standard solution Substances 0.000 claims 1
- 238000002386 leaching Methods 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000976 ink Substances 0.000 description 47
- 235000019504 cigarettes Nutrition 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 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
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010812 external standard method Methods 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- -1 link stuff Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 238000004176 ammonification Methods 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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
Abstract
The present invention provides a kind of detection method of ammonia content in tipping paper water-based ink using ion chromatography.Specifically weigh M1G water-based ink samples add its v1ML acid solutions extract, and take out container and place to upper liquid clarification, further take out v2The clarification of mL upper liquids filters water-based gloss oil using ultrafiltration membrane, after filtering, uses M2The ultra-pure water cleaning filter membranes of g, collect filtrate and cleaning solution, and pipette 5mL filtrates and cleaning solution pressurizeed C18Solid phase microextraction column, eluted by several times for 0.005~0.01mol/L Loprazolams or sulfuric acid acid solution with 15.0mL concentration again, collect filtrate and washing lotion obtains testing sample solution, analysis detection is carried out using ion chromatograph, and ammonia content C in testing sample solution is calculated by standard curve, finally it is multiplied by corresponding extension rate and obtains final ammonia content.Detection process of the present invention is quick and convenient, its detection level result is accurate, high sensitivity.
Description
Technical field
The present invention relates to by the small molecule component to the water-based ink used in cigarette tipping paper and macromolecular substances into
Row separation and its ion chromatography detection method of ammonia content quantitative analysis.
Background technology
The quality of cigarette tipping paper directly influences the experience of consumer, therefore is gradually paid attention to by everybody.In recent years, by
In the enhancing of people's health consciousness, the production technology of cigarette tipping paper has been greatly improved, for example with alcohol-soluble printing ink
Printed instead of ester soluble ink, punched on tipping paper to dilute harmful components in main flume etc..
The same with other printing ink, water-based ink main component includes colorant, link stuff, solvent and auxiliary agent.Only will
The ratio of ink each component is deployed, can be only achieved the due printability of ink and performance, can just make printing ink with
Good cooperation is able between printing plate, printing machine, printable fabric, is smoothed out typography.
Auxiliary agent is also additive, is the auxiliary element of ink, its act on be adjust ink printability, in order not to
Purpose, will add variety classes and the auxiliary agent of quantity, to adjust the mobility of ink, drying property, tone in the preparation of ink
Deng.The physical and chemical performance of water-based ink is largely determined by the additive in water-based ink.Additive is added into ink,
It is conventional means in flexographic printing industry to obtain some specific physical and chemical performances.In water-based ink, colorant, resin and molten
Agent accounts for the 95% of ink composition, remaining 5% is various additives.They include (1) lubricant, (2) surfactant,
(3) crosslinking agent, (4) adhesion promoter, (5) defoamer, (6) fungicide, (7) ore deposit material, (8) oxidant, (9) plasticizer.
Ore deposit material wherein in water-based ink, is typically ammonium hydroxide, with dissolving resin link stuff, can keep the pH of water-based ink stabilization
Value, while also ensure the printability of water-based ink.Research afterwards finds that the chemical property of ammonia is very unstable, and spinosity
Nose smell, so part amine compounds used for water color ink replace, their stability is better, but likewise suffers to volume
The hidden danger of cigarette sense organ negative effect.
Tobacco business it is most crucial be no more than cigarette product, they to Sensory Quality of Cigarette require it is very stringent.But tobacco
Whether industry tipping paper production division usually detects in material VOC content with national standard YC 263-2014 and YC 171-2014 etc.
It is restricted to the auxiliary agent of addition in security and require to meet standard, but this detection is more focused on the investigation of security risk,
There is no considered critical to the content of ammonia, so that the wind that auxiliary material brings negative effect to cigarette product suction organoleptic quality can not be eliminated
Dangerous hidden danger.
, generally can not direct injected gas-chromatography also, water-based ink contains water；Macromolecule resin, viscosity is larger, boiling point
It is higher, there are some hardly possible volatilization impurity, also unsuitable direct injected chromatography, can pollute instrument component, head space equipment can not be complete
The accurate quantitative analysis of ammonification.Common detection methods are without reference to, it is necessary to which pretreatment technology assists ion chromatography to detect water-based oil
Ammonia in ink.
The content of the invention
There is provided it is an object of the invention to deficiency according to prior art a kind of water-based using ion chromatography tipping paper
The detection method of ammonia content in ink, the present invention is in utilization molecule filter membrane Selective Separation small molecule and macromolecular components；Small point
Subgroup point can the various chromatographs of direct injected, including ion chromatograph detection.Analyzed by quantified by external standard method, instrument will not be caused
Component contamination, the concrete content of ammonia is quantitatively detected using ion chromatography.
Technical solution provided by the invention in view of the deficiencies of the prior art：One kind is water-based using ion chromatography tipping paper
The detection method of ammonia content in ink, it is characterised in that comprise the following steps that：
(1) precise M1G water-based ink samples, are placed in container, add its v1ML acid solutions be placed in oscillator with 160~
200R/min speed oscillations are extracted for 5~8 minutes, after extraction is completed, are taken out container and are placed to upper liquid clarification；Wherein water
Property ink sample mass M1For 5~20g, acid solution amount v is added1For 5~10mL；
(2) supernatant liquor in step (1) is accurately taken out into v2ML, filters water-based ink using ultrafiltration membrane, operation pressure
For 1.5 × 105Pa~3.0 × 105Pa, the average pore size for selecting film are 0.1~0.4 μm；After filtering, M is used2The ultra-pure water cleaning of g
Filter membrane, collects merging by filtered fluid and cleaning solution and obtains water-based ink solution；Its water-based ink sample quality M1With it is super
Pure water mass M2Meet following relation：M1<M2<10M1；The supernatant liquor amount v taken out in step (1)2For 5.0~10.0mL,
Extension rate caused by filtering is (M1+M2)v1/M1v2；
(3) the accurate water-based ink solution 5.0mL pipetted after filtering, pressurizeed C18Solid phase microextraction column, keeps flow velocity
0.5~2mL/ minutes, then eluted by several times for 0.005~0.01mol/L Loprazolams or sulfuric acid acid solution with 15.0mL concentration, collect
Filtrate and washing lotion, obtain testing sample solution after mixing, wherein described cross C18Extension rate caused by solid phase microextraction column
For 4 times；
(4) sulfuric acid solution for being 0.005mol/L with concentration prepares the ammonia standard working solution of various concentrations, and uses ion
Chromatography standard solution, draws the standard curve of tested component, and a coordinate of the standard curve is the mark of tested component
Quasi- thing concentration, another coordinate are that the reference material of tested component corresponds to the peak area at peak；
(5) analysis detection is carried out to testing sample solution in step (3) using ion chromatograph, obtains related chromatogram,
And calculate NH+ 4Peak area, ammonia content in testing sample solution is then calculated by the standard curve obtained in step (4)
C, and it was multiplied by C18Extension rate caused by extension rate caused by solid phase microextraction column is 4 times and filters is (M1+M2)v1/
M1v2It is as follows to calculate total ammonia amount M, its calculation formula in water-based ink sample：
M=4Cv1·(M1+M2)/(v2·M1) (1)
Wherein M-total ammonia content, mg/L；C-ammonia content measured value, mg/L；M1- water-based ink sample quality, g；M2—
Ultrapure water quality, g used in cleaning filter membranes；v1- extraction acid solution volume, mL；v2- pipette extract volume, mL；
The chromatographic column of the ion chromatography uses Dionex IonPacTMCS19 or CS12A chromatographic columns, 4mm ×
250mm；Leacheate：Loprazolam solution；Flow velocity：1.0mL/min；Sample size：10~30 μ L；Column temperature：30~40 DEG C；Detector
Chi Wen：35~50 DEG C.
The present invention preferably technical solution：Acid solution in the step (1) is 0.005~0.02mol/L's of mass concentration
Loprazolam or sulfuric acid.
The present invention preferably technical solution：The standard solution of preparation is respectively in the step (4)：0.01mg/L、
0.05mg/L, 0.2mg/L, 0.6mg/L, 2.0mg/L Pyatyi ammonia standard solution.
Standard ammoniacal liquor in the present invention, ammonia standard solution；Acid solution：Loprazolam, sulfuric acid solution；Filter membrane leacheate：It is ultrapure
Water.
This hair utilizes ultrafiltration membrane, Selective Separation water-based ink low molecular weight impurities component (including ammonia, ethanol, acetone, etc.
Deng), macromolecular components (including soluble resin etc.)；Pass through C18 solid phase microextraction column purifications again, emphasis is collected to organoleptic quality
Related ammonia components, make ion chromatography become feasible method, lift the accuracy of subsequent detection.For directly using top
Empty string connection GC-MS instrument and gas phase flame ionization ditector (GC-FID) do not measure, indeterminable object ammonia, this method
It can complete detection work；Ammonia content detection can be completed by isolation technics, sample direct injected ion chromatography.
The present invention is separated the volatile component of water-based ink sample by ultrafiltration membrane, is eliminated macromolecular substances and is done
Disturb, can relatively detect the component that some conventional methods can not be detected accurately, reduce detection error, eliminate viscosity higher molecular weight
Larger material interference, can direct injected ion chromatography, and heating schedule and chromatographic column are required to reduce, detection process is fast
Speed is convenient, its detection level result is accurate, high sensitivity.
Brief description of the drawings
Fig. 1 is the canonical plotting in embodiment.
Specific implementation method
In order to further appreciate that the present invention, the preferred embodiment of the invention is described with reference to embodiment.
The present invention is to add a small amount of sulfuric acid or methanesulfonic acid as extract, by Ultra filtration membrane volatile component and higher
Boiling point component；Solvent dosage is smaller, plays the effect to target analytes separation and concentration；External standard method direct injected ion chromatograph
Detect volatile component content.Should meet can be with the basic demand of direct injected ion chromatograph for solvent in the present invention；Solvent is
The low-boiling point material being not present in sample to be tested；Solvent and tested component intermiscibility are preferable, but polarity difference cannot be too close, with
Solvent chromatographic peak is set to be kept completely separate with tested component chromatographic peak；Solvent cannot be chemically reacted with component to be measured.Therefore it is molten
Agent is preferably ultra-pure water or acid solution.
The preferred embodiment of the present invention is as follows：
Embodiment 1 is as follows for the detection of ammonia content in four kinds of kinds of cigarettes tipping paper water-based inks, its detailed process：
(1) sample pre-treatments and purifying：Pin precise M respectively1Tetra- kinds of water-based ink samples of g, are placed in into ground taper
In bottle, its v is added1ML concentration is placed on oscillator for the molten capping of 0.01mol/L Loprazolams and is divided with 160R/min speed oscillations 6
Clock；Take out conical flask and place to upper liquid the supernatant liquid for clarifying four kinds of water-based ink samples of collection；Wherein, four kinds of water-based oil
Black sample quality M1With acid solution amount v11 is shown in Table respectively；
(2) supernatant liquid of four kinds of water-based ink samples in step (1) is accurately taken out into v respectively2ML, utilizes ultrafiltration
Film filters water-based ink, and operating pressure is 2 × 105Pa, the average pore size for selecting film are 0.3 μm；After filtering, M is used2G's is ultrapure
Water cleaning filter membranes, collect merging by filtered fluid and cleaning solution and obtain four kinds of water-based ink sample solutions；Its water-based ink
Sample quality M1With ultra-pure water mass M2Meet following relation：0.5M1<M2<5M1；Extension rate caused by filtering is (M1+M2)v1/
M1v2；The cleaning solvent mass M of four kinds of water-based ink samples2With supernatant liquor amount v21 is shown in Table respectively；
Table 1 weighs each parameter of sample and is diluted ratio
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | |
| Water-based ink M1(g) | 9.431 | 5.996 | 2.154 | 9.882 |
| Ultra-pure 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) the accurate four kinds of water-based ink sample solutions pipetted in 5mL steps (2), pressurizeed C18Solid phase microextraction column, makes
Flow velocity is kept for 1~5mL/ minutes；It is again that 0.01mol/L Loprazolams elute by several times with 15.0mL concentration, collects filtrate and washing lotion,
Testing sample solution is obtained after mixing, wherein described cross C18Extension rate caused by solid phase microextraction column is 4 times；
(4) chromatographic column of the ion chromatography uses Dionex IonPacTMCS19 or CS12A chromatographic columns, 4mm ×
250mm；Leacheate：Loprazolam solution；Flow velocity：2.0mL/min；Sample size：20μL；Column temperature：35℃；Detector cell temperature：45
DEG C,
Gradient condition：
Leacheate gradient elution program
(5) standard curve is drawn：It is fixed molten with 0.005mol/L sulfuric acid solutions, standard curve concentration is 0.011,0.049,
0.205th, 0.597,2.034mg/L, by Pyatyi titer according to the ion chromatography condition in step (4) respectively into ion chromatograph
Analyzed, each tested component respective standard curve is obtained, as shown in Figure 1, linear fit equation form is Y=aX+b；It is described
One coordinate of standard curve is the reference material concentration of tested component, another coordinate is that the reference material of tested component corresponds to peak
Product peak area；By each object one to Pyatyi standard liquid sample introduction ion chromatography, draw calibration curve equation formula and be listed in table 2.
The calibration curve equation formula that each tested component GC-MS of table 2 is analyzed
| Object | Standard curve | Relative deviation R |
| Ammonia | Y=0.488X+0.152 | 0.99995 |
Remarks：X is the peak area that object corresponds to peak；Y is target concentration (mg/L)
(6) analysis detection is carried out to testing sample solution in step (3) using ion chromatograph, ion chromatography condition is as walked
Suddenly (4), obtain related chromatogram, and calculate NH+ 4Peak area, then calculated by the standard curve that is obtained in step (5)
Go out ammonia content C in testing sample solution, and total ammonia amount M in each water-based gloss oil sample is calculated according to following calculation formula：
M=4Cv1·(M1+M2)/(v2·M1) (1)
Wherein M-total ammonia content, mg/L；C-ammonia content measured value, mg/L；M1- water-based ink sample quality, g；M2—
Ultrapure water quality, g used in cleaning filter membranes；v1- extraction acid solution volume, mL；v2- pipette extract volume, mL；
It is as shown in table 3 to test and analyze to obtain sample ammonia content through ion chromatograph,
3 ammonia testing result of table
By technical method provided by the invention, ammonia content in four samples is detected, and according to this content be according to
According to providing judge to the qualified or not of supplier's product.For example, No. 1, No. 2 ammonia contents of sample are relatively low, therefore the standard is qualified；And
Sample 4, ammonia content is excessive, limits the quantity, is judged as unqualified beyond inner quality standard.The present invention is lifting tipping paper product quality
Provide important guarantee.
Claims (3)
- A kind of 1. detection method of ammonia content in tipping paper water-based ink using ion chromatography, it is characterised in that specific steps It is as follows：(1) precise M1G water-based ink samples, are placed in container, add its v1ML acid solutions are placed in oscillator with 160~200R/ Min speed oscillations are extracted for 5~8 minutes, after extraction is completed, are taken out container and are placed to upper liquid clarification；Wherein water-based oil Black sample quality M1For 5~20g, acid solution amount v is added1For 5~10mL；(2) supernatant liquor in step (1) is accurately taken out into v2ML, filters water-based ink using ultrafiltration membrane, operation pressure is 1.5 ×105Pa~3.0 × 105Pa, the average pore size for selecting film are 0.1~0.4 μm；After filtering, M is used2The ultra-pure water cleaning filter membranes of g, Filtered fluid and cleaning solution are collected into merging and obtain water-based ink solution；Its water-based ink sample quality M1With ultrapure water quality Measure M2Meet following relation：M1<M2<10M1；The supernatant liquor amount v taken out in step (1)2For 5.0~10.0mL, filtering is made Into extension rate be (M1+M2)v1/M1v2；(3) the accurate water-based ink solution 5.0mL pipetted after filtering, pressurizeed C18Solid phase microextraction column, make flow velocity keep 0.5~ 2mL/ minutes, then eluted by several times for 0.005~0.01mol/L Loprazolams or sulfuric acid acid solution with 15.0mL concentration, collect filtrate And washing lotion, testing sample solution is obtained after mixing, wherein described cross C18Extension rate caused by solid phase microextraction column is 4 Times；(4) sulfuric acid solution for being 0.005mol/L with concentration prepares the ammonia standard working solution of various concentrations, and uses ion chromatography Analytical standard solution, draws the standard curve of tested component, and a coordinate of the standard curve is the reference material of tested component Concentration, another coordinate are that the reference material of tested component corresponds to the peak area at peak；(5) analysis detection is carried out to testing sample solution in step (3) using ion chromatograph, obtains related chromatogram, and count Calculate NH+ 4Peak area, ammonia content C in testing sample solution is then calculated by the standard curve obtained in step (4), and It was multiplied by C18Extension rate caused by extension rate caused by solid phase microextraction column is 4 times and filters is (M1+M2)v1/M1v2Meter It is as follows to calculate total ammonia amount M, its calculation formula in water-based ink sample：M=4Cv1·(M1+M2)/(v2·M1) (1)Wherein M-total ammonia content, mg/L；C-ammonia content measured value, mg/L；M1- water-based ink sample quality, g；M2- cleaning Ultrapure water quality, g used in filter membrane；v1- extraction acid solution volume, mL；v2- pipette extract volume, mL；The chromatographic column of the ion chromatography uses Dionex IonPacTMCS19 or CS12A chromatographic columns, 4mm × 250mm；Leaching Washing lotion：Loprazolam solution；Flow velocity：1.0mL/min；Sample size：10~30 μ L；Column temperature：30~40 DEG C；Detector cell temperature：35 ~50 DEG C.
- 2. the detection side of ammonia content in a kind of tipping paper water-based ink using ion chromatography according to claim 1 Method, it is characterised in that：The Loprazolam or sulfuric acid that acid solution in the step (1) is 0.005~0.02mol/L of mass concentration.
- 3. the detection side of ammonia content in a kind of tipping paper water-based ink using ion chromatography according to claim 1 Method, it is characterised in that：The standard solution of preparation is respectively in the step (4)：0.01mg/L、0.05mg/L、0.2mg/L、 0.6mg/L, 2.0mg/L Pyatyi ammonia standard solution.
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Cited By (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 |
| CN112326856A (en) * | 2020-12-01 | 2021-02-05 | 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)
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| CN112326856A (en) * | 2020-12-01 | 2021-02-05 | 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 |
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| CN108037215B (en) | 2020-09-08 |
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