CN108195966A - The detection method of ammonia content in a kind of cigarette tipping paper water-based gloss oil - Google Patents
The detection method of ammonia content in a kind of cigarette tipping paper water-based gloss oil Download PDFInfo
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- CN108195966A CN108195966A CN201810017937.8A CN201810017937A CN108195966A CN 108195966 A CN108195966 A CN 108195966A CN 201810017937 A CN201810017937 A CN 201810017937A CN 108195966 A CN108195966 A CN 108195966A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 44
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 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
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 9
- 239000012498 ultrapure water Substances 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 7
- 238000004458 analytical method Methods 0.000 claims abstract description 5
- 238000005352 clarification Methods 0.000 claims abstract description 4
- 239000006210 lotion Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 30
- 239000000523 sample Substances 0.000 claims description 29
- 238000004255 ion exchange chromatography Methods 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 5
- 239000013558 reference substance Substances 0.000 claims description 5
- 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 4
- 229960003019 loprazolam Drugs 0.000 claims description 4
- 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
- 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 2
- 239000012224 working solution Substances 0.000 claims description 2
- 239000002387 analytical standard solution Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 42
- 239000002904 solvent Substances 0.000 description 14
- 239000012752 auxiliary agent Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- -1 drier Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010812 external standard method Methods 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000009736 wetting Methods 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
-
- 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
- G01N30/96—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 using ion-exchange
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- 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)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention provides a kind of detection method of ammonia content in cigarette tipping paper water-based gloss oil.Specifically weigh M1G water-based gloss oil samples add in 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 v3ML filtrates and cleaning solution pressurizeed C18Solid phase microextraction column, it is eluted by several times with a concentration of 0.005~0.01mol/L Loprazolams of 10.0mL or sulfuric acid acid solution again, it collects filtrate and washing lotion obtains testing sample solution, analysis detection is carried out using ion chromatograph, and pass through standard curve and calculate ammonia content C in testing sample solution, it is finally multiplied by corresponding extension rate and obtains final ammonia content.Detection process of the present invention is quick and convenient, and detection level result is accurate, high sensitivity.
Description
Technical field
The present invention relates to the detection of ammonia content in water-based gloss oil, ammonia content in specifically a kind of cigarette tipping paper water-based gloss oil
Detection method.
Background technology
Water-based gloss oil is mainly made of host agent, solvent, adjuvant three categories, has colourless, and tasteless, transparent feel is strong and nothing
Poison, without organic volatile, at low cost, the features such as source is wide, other solvent borne oil polishes can not be compared.If add in it
Its host agent and auxiliary agent, can also have good glossiness, wearability and chemical resistance, and economic health is outstanding to packages printing
It is suitable.Due to its superior characteristic, tobacco business also can extensive use, such as box piece, tipping paper printing ink etc..
The host agent of water lustering oil is film-forming resin, is the film forming matter of glazing agent, is generally synthetic resin, it influence and
Support the various physical properties of deep layer and the glazing quality of film layer, such as glossiness, adhesion, drying property.Solvent it is main
Effect is to disperse or dissolve synthetic resin, various auxiliary agents.The solvent of water lustering oil is mainly water.The volatility of water is almost
Zero, flow leveling is very good.But water also has shortcoming as the solvent of water lustering oil, as rate of drying is relatively slow, holds
Easily cause the unstable grade technology troubles of product size.This just needs to add various auxiliary agents to improve the physicochemical property of waterborne glazing agent
And processing characteristics.The type of auxiliary agent have including curing agent, surfactant, the sour agent (alkaline matter) of control, antifoaming agent, drier,
Adhesion promoter, wetting dispersing agent and plasticizer etc..Also, usually restricted to the auxiliary agent of addition only in safety and requirement, it is right
Whether limited in detail with odorous nothing.
Tipping paper printing ink is numerous using water-based gloss oil type and specification, it is desirable that and addition auxiliary agent is also diversified.Similary title
Raw material may it is different due to production method, production technology is different, main component is different, producer's packing storage is different etc., cause
Impurity is different, and there are different degrees of hidden danger.Tobacco business is mostly used national standard YC 263-2014 and YC 171-2014 etc. to detect
Whether VOC content complies with standard in material.But this detects the investigation for being more focused on security risk, hidden to odoring substance and sense organ
Suffer from no considered critical, the risk hidden danger of negative effect is brought so as to which auxiliary material can not be eliminated to cigarette product suction organoleptic quality.
In order to promote the performances such as the applicability of water-based gloss oil, a variety of auxiliary agents can be added, some of which contains ammonia, needs to be examined with ion chromatography
The ammonia in aqueous solution is surveyed, but water-based gloss oil contains water, macromolecule resin, viscosity is larger, boiling point is higher, also some hardly possible volatilizations
Impurity, also unsuitable direct injected chromatography.
Invention content
It is an object of the invention to for water-based gloss oil used in cigarette tipping paper ink, its ammonia content is examined
It surveys, specifically utilizes molecule filter membrane Selective Separation small molecule and macromolecular components；Small molecule component can the various colors of direct injected
Spectrometer is detected including ion chromatograph.It is analyzed by quantified by external standard method, instrument component will not be caused to pollute, utilize ion chromatography
Quantitatively detect the concrete content of ammonia.
The present invention provides a kind of detection method of ammonia content in cigarette tipping paper water-based gloss oil, it is characterised in that specific steps
It is as follows：
(1) precise M1G water-based gloss oil samples, are placed in container, add in its v1ML acid solutions are placed on 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 gloss oil sample quality M1For 5~20g, acid solution amount v is added in1For 5~20mL；
(2) supernatant liquor in step (1) is accurately taken out into v2ML filters water-based gloss oil using ultrafiltration membrane, operation pressure
It is 1.5 × 105Pa~5.0 × 105Pa, the average pore size for selecting film are 20~100 angstroms；After filtering, M is used2The ultra-pure water cleaning of g
Filtered fluid and cleaning solution are collected merging and obtain water-based gloss oil solution by filter membrane；Its water-based gloss oil sample quality M1With it is super
Pure water mass M2Meet following relationship：0.5M1<M2<5M1；The supernatant liquor amount v taken out in step (1)2For 2.0~
5.0mL, extension rate caused by filtering are (M1+M2)v1/M1v2；
(3) v is accurately pipetted3Water-based gloss oil solution in mL steps (2), pressurizeed C18Solid phase microextraction column protects flow velocity
It holds 1~5mL/ minutes, the amount of the pipetting v of the water-based gloss oil solution1For 5.0~10.0mL；Again with 10.0mL a concentration of 0.005~
0.01mol/L Loprazolams or sulfuric acid acid solution elute by several times, collect filtrate and washing lotion, it is molten to obtain sample to be tested after mixing
Liquid, wherein described cross C18Extension rate caused by solid phase microextraction column is (v3+10)/v3；
(4) the ammonia standard working solution of various concentration is prepared with the sulfuric acid solution of a concentration of 0.005mol/L, 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- object concentration, another coordinate are that the reference substance 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 solid phase microextraction column is (v3+10)/v3It is (M with extension rate caused by filtering1+
M2)v1/M1v2It is as follows to calculate total ammonia amount M, calculation formula in water-based gloss oil sample：
M=Cv1(v3+10)·(M1+M2)/(v2·v3·M1) (1)
Wherein M-total ammonia content, mg/L；C-ammonia content measured value, mg/L；M1- water-based gloss oil sample quality, g；M2—
Ultrapure water quality, g used in cleaning filter membranes；v1- extraction acid solution volume, mL；v2- pipette extract liquor volume, mL；v3- pipette filter
Liquid accumulates, 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：20~30 μ L；Column temperature：30~40 DEG C；Detector
Chi Wen：35~50 DEG C,
Gradient condition：
Leacheate gradient elution program
Preferably technical solution of the invention is：The first for being 0.005~0.02mol/L of mass concentration in the step (1)
Alkyl sulfonic acid or sulfuric acid acid solution.
Preferably technical solution of the invention is：The standard solution of preparation is respectively in the step (4)：0.05mg/L,
0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L Pyatyi ammonia standard solution.
The present invention using ultrafiltration membrane, Selective Separation water-based gloss oil low molecular weight impurities component (including ammonia, methanol, acetone,
Isopropanol, methyl methacrylate, methyl acrylate, ethyl acetate, benzene, toluene, styrene, ethylbenzene, dimethylbenzene, etc.), it is big
Molecular components (including resins synthesis by-product and macromolecular resin etc.)；Using C18 solid phase microextraction column purifications, emphasis is collected
The related ammonia components to organoleptic quality make ion chromatography become feasible method, promote the accuracy of subsequent detection.For
It is not measured using head space series connection GC-MS instrument and gas phase flame ionization ditector (GC-FID) directly, indeterminable target
Object ammonia, this method can complete detection work；Can ammonia detection be completed by isolation technics, sample direct injected ion chromatography.
The present invention is separated the volatile component of water-based gloss oil sample by ultrafiltration membrane, is eliminated macromolecular substances and is done
It disturbs, can relatively detect the component that some conventional methods can not be detected accurately, reduce detection error, eliminate viscosity higher molecular weight
Larger substance interference, can direct injected ion chromatography, and temperature program and chromatographic column requirement are reduced, detection process is fast
Speed is convenient, and detection level result is accurate, high sensitivity.
Description of the drawings
Fig. 1 is the ammonium ion chromatogram of water-based gloss oil sample 1；
Fig. 2 is the ammonium ion chromatogram of water-based gloss oil sample 2；
Fig. 3 is the ammonium ion chromatogram of water-based gloss oil sample 3；
Fig. 4 is the ammonium ion chromatogram of water-based gloss oil sample 4.
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 be add on a small quantity will not the property sent out acid as extract liquor and solvent, by Ultra filtration membrane volatile component and
Higher component；Solvent dosage is smaller, plays the effect isolated and purified to target analytes；External standard method direct injected ion color
Spectrometer detects the content of ammonia.Should meet can be with the basic demand of direct injected ion chromatograph for solvent in the present invention；Solvent is treats
The low-boiling point material being not present in sample；Solvent and tested component intermiscibility are preferable, but polarity difference cannot be too close, so that
Solvent chromatographic peak can be kept completely separate with tested component chromatographic peak；Solvent cannot be chemically reacted with component to be measured.Therefore solvent
Preferably ultra-pure water or acid solution.
The preferred embodiment of the present invention is as follows：
Embodiment 1, for the detection of ammonia content in four kinds of kinds of cigarettes tipping paper water-based gloss oils, detailed process is as follows：
(1) sample pre-treatments and purifying：Needle precise M respectively1Tetra- kinds of water-based gloss oil samples of g, are placed in conical flask, add
Enter its v1The molten oscillator that is placed in of a concentration of 0.01mol/L Loprazolams of mL is extracted for 5 minutes with 160R/min speed oscillations, extraction
It takes into later, takes out conical flask and place to upper liquid the supernatant liquid for clarifying four kinds of water-based gloss oil samples of collection；Wherein, four
Kind water-based gloss oil sample quality M1With acid solution amount v1It is shown in Table 1 respectively；
(2) supernatant liquid of four kinds of water-based gloss oil samples in step (1) is accurately taken out into v respectively2ML utilizes ultrafiltration
Film filters water-based gloss oil, and operating pressure is 1.5 × 105Pa, the average pore size for selecting film are 50 angstroms；After filtering, M is used2G's is super
Filtered fluid and cleaning solution are collected merging and obtain four kinds of water-based gloss oil sample solutions by pure water cleaning filter membranes；Its aqueous light
Oil samples mass M1With ultra-pure water mass M2Meet following relationship：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 gloss oil samples2With supernatant liquor amount v2It is shown in Table 1 respectively；
(3) v is accurately pipetted3Four kinds of water-based gloss oil sample solutions in mL steps (2), pressurizeed C18Solid phase microextraction column,
Flow velocity is made to be kept for 1~5mL/ minutes, the amount of the pipetting v of the water-based gloss oil solution3For 5.0~10.0mL；10.0mL concentration is used again
It is eluted by several times for 0.01mol/L Loprazolams, collects filtrate and washing lotion, obtain testing sample solution after mixing, wherein institute
Stated C18Extension rate caused by solid phase microextraction column is (v3+10)/v3；The amount of pipetting of four kinds of water-based gloss oil sample solutions
v3Refer to table 1：
Table 1 weighs each parameter of sample and is diluted ratio
(4) the ion chromatographic separation condition of ion chromatography instrument is set：Dionex IonPacTMCS19 or CS12A chromatographies
Column：4mm×250mm；Leacheate：Loprazolam or sulfuric acid solution；Flow velocity：2.0mL/min；Sample size：20μL；Column temperature：35℃；
Detector cell temperature：50℃；
Gradient condition：
Leacheate gradient elution program
(5) standard curve is drawn：Pyatyi ammonia standard solution is configured, standard curve is a concentration of 0.049,0.101,0.204,
0.497th, 1.026mg/L is divided Pyatyi titer according to the ion chromatography condition in step (4) into ion chromatograph respectively
Analysis, obtains each tested component respective standard curve, and linear fit equation form is Y=aX+b；One seat of the standard curve
The reference substance concentration of tested component is designated as, another coordinate is that the reference substance of tested component corresponds to the product peak area at peak；By each
The one of object draws calibration curve equation formula and is listed in table 2 to Pyatyi standard liquid sample introduction ion chromatography.
The calibration curve equation formula that each tested component GC-MS of table 2 is analyzed
| Object | Standard curve | Relative deviation R |
| Ammonia | Y=0.731X-1.063 | 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 as shown in Figures 1 to 4, and calculate NH+ 4Peak area, then by being obtained in step (5)
Standard curve calculate ammonia content C in testing sample solution, and each water-based gloss oil sample is calculated according to following calculation formula
Total ammonia amount M, calculation formula are as follows in product：
M=Cv1(v3+10)·(M1+M2)/(v2·v3·M1) (1)
Wherein M-total ammonia content, mg/L；C-ammonia content measured value, mg/L；M1- water-based gloss oil sample quality, g；M2—
Ultrapure water quality, g used in cleaning filter membranes；v1- extraction acid solution volume, mL；v2- pipette extract liquor volume, mL；v3- pipette filter
Liquid accumulates, mL；
Its result of calculation is as shown in table 3：
3 ammonia testing result of table
By technical method provided by the invention, ammonia content in four samples detected, and according to this content be according to
According to providing judge to the qualified or not of supplier's product.For example, sample 4 does not detect ammonia, No. 1 ammonia content of sample is relatively low,
Therefore the standard is qualified；And sample 3, ammonia content are higher, have exceeded inner quality standard limitation, are judged as unqualified.The present invention is carries
It rises tipping paper product quality and provides important guarantee.
Claims (3)
1. the detection method of ammonia content in a kind of cigarette tipping paper water-based gloss oil, it is characterised in that be as follows：
(1) precise M1G water-based gloss oil samples, are placed in container, add in its v1ML acid solutions be placed on 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 gloss oil sample quality M1For 5~20g, acid solution amount v is added in1For 5~20mL；
(2) supernatant liquor in step (1) is accurately taken out into v2ML filters water-based gloss oil using ultrafiltration membrane, and operation pressure is 1.5
×105Pa~5.0 × 105Pa, the average pore size for selecting film are 20~100 angstroms；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 gloss oil solution；Its water-based gloss oil sample quality M1With ultrapure water quality
Measure M2Meet following relationship：0.5M1<M2<5M1；The supernatant liquor amount v taken out in step (1)2For 2.0~5.0mL, filtering
Caused by extension rate be (M1+M2)v1/M1v2；
(3) v is accurately pipetted3Water-based gloss oil solution in mL steps (2), pressurizeed C18Solid phase microextraction column, make flow velocity keep 1~
5mL/ minutes, the amount of the pipetting v of the water-based gloss oil solution1For 5.0~10.0mL；Again with 10.0mL a concentration of 0.005~
0.01mol/L Loprazolams or sulfuric acid acid solution elute by several times, collect filtrate and washing lotion, it is molten to obtain sample to be tested after mixing
Liquid, wherein described cross C18Extension rate caused by solid phase microextraction column is (v3+10)/v3；
(4) the ammonia standard working solution of various concentration is prepared with the sulfuric acid solution of a concentration of 0.005mol/L, and uses ion chromatography
Analytical standard solution, draws the standard curve of tested component, and a coordinate of the standard curve is the reference substance of tested component
Concentration, another coordinate are that the reference substance 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 solid phase microextraction column is (v3+10)/v3It is (M with extension rate caused by filtering1+M2)v1/
M1v2It is as follows to calculate total ammonia amount M, calculation formula in water-based gloss oil sample：
M=Cv1(v3+10)·(M1+M2)/(v2·v3·M1) (1)
Wherein M-total ammonia content, mg/L；C-ammonia content measured value, mg/L；M1- water-based gloss oil sample quality, g；M2- cleaning
Ultrapure water quality, g used in filter membrane；v1- extraction acid solution volume, mL；v2- pipette extract liquor volume, mL；v3- pipette filtrate body
Product, 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：20~30 μ L；Column temperature：30~40 DEG C；Detector cell temperature：
35~50 DEG C.
2. the detection method of ammonia content in a kind of cigarette tipping paper water-based gloss oil according to claim 1, it is characterised in that：
The Loprazolam or sulfuric acid acid solution that are 0.005~0.02mol/L of mass concentration in the step (1).
3. the detection method of ammonia content in a kind of cigarette tipping paper water-based gloss oil according to claim 1, it is characterised in that：
The standard solution of preparation is respectively in the step (4)：0.05mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L five
Grade ammonia standard solution.
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