CN101059497A - Method for identifying oil-soluble printing oil/ printing mud writing relative formation time - Google Patents
Method for identifying oil-soluble printing oil/ printing mud writing relative formation time Download PDFInfo
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- CN101059497A CN101059497A CN 200710078489 CN200710078489A CN101059497A CN 101059497 A CN101059497 A CN 101059497A CN 200710078489 CN200710078489 CN 200710078489 CN 200710078489 A CN200710078489 A CN 200710078489A CN 101059497 A CN101059497 A CN 101059497A
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Abstract
The invention provides a method for checking the forming time of oil soluble stamp-pad ink or stamp pad, characterized in that parallel checking the solubility of object pad and reference sample pad, comparing to judge the forming time. The invention has simple operation, reliable and accurate result, with wide application in the forming time check of oil soluble stamp-pad ink or stamp pad. The invention can check the forming time of oil soluble stamp-pad ink or stamp pad in three years, with reference sample.
Description
Technical field
The present invention relates to the chemical analysis of forensic science material evidence, specifically a kind of oil-soluble stamp-pad ink or ink paste seal literary composition method of formation time relatively of identifying.
Background technology
Deep development along with market economy, people's social interaction is increased, contact document each other is more and more, the case of the forgery of Chan Shenging thereupon, adulterium document is obvious ascendant trend, little of individual's debt-credit among the people, divorce properties division, testament dispute etc., big to corruption, great economy swindle, the loss of state-owned assets etc.In all kinds of punishment, civil case, usually in this case, the actual time of making of suspicious document has just become to identify the important evidence of the document true and false to the litigant to reach certain purpose Production Time of document forgery.And in view of the effect of seal impression proof identity and credit, the lawless person has often also added a cover simultaneously Yin Wen in order to reach its illegal objective on suspicious document, have great meaning so print the evaluation of civilian formation time.
The difficult problem that the research institute of printing civilian formation time is run into has: after 1, Yin Wen was formed on the carrier, the influence of preservation condition was uncertain; 2, the carrier material of impressing is uncertain to the influence of ink paste or stamp-pad ink composition; 3, the influence of ink paste (oil) kind is uncertain; 4, the condition effect of impressing is uncertain.These uncertain factors have hindered the progress of research work.At present, determining to mainly contain following technical method on the civilian formation time of seal: (1) is grasped the seal literary composition and is lasted Changing Pattern and determine the time of impressing by printing civilian conditions of the current stage; Promptly mainly print civilian sample and the comparison of sample seal literary composition by collecting each stage.Some variation meetings that seal in use takes place reflect in the document of different times, the local damage that causes as mechanical force, repair feature and hard particles is stuck or block ink paste is adhered to the features such as fault, patch of formation, the appearance of these features can become and judge that sample prints the foundation of civilian formation time.This method shortcoming is, the sample that lasts of seal literary composition usually is difficult to collect, and that the seal literary composition is gone up is damaged, the origin cause of formation of fault, patch is difficult to judge.(2) determine the time of impressing by the check of red and black sequential; Be to have the literal of the time of can determining and sample to print civilian juxtaposition on the suspicious document, the upper limit or the lower limit that sample seal literary composition forms determined in the check that forms sequencing by literal and seal literary composition.This method shortcoming is, is only limited to the situation of red and black juxtaposition, and can determines the time with the position literal, and in addition, the judgement of red and black sequential in most cases difficulty is also bigger, so accuracy rate is also low.(3) ooze the degree of loosing by the civilian oil trace of mensuration seal and determine the time of impressing; Promptly loose speed from fast to slow, and final no longer diffusion reaches stable principle and implements check according to oil trace oozing on carrier (paper) in the seal literary composition.The method is easy to be suitable for, and does not need sample, higher to the testing accuracy that forms the seal literary composition in the near future below 3 months.Maximum limitation is to be used for the impress check of literary composition of in the check days 3 months institute, and civilian powerless to seal more than 3 months, and in the actual case suspicious document time debatable all at this moment between outside the scope.In a word, because the limitation of prior art, up to the present, still none accurate, reliable, easy method of inspection is identified the formation time of common ink paste or stamp-pad ink seal literary composition.
Summary of the invention
Purpose of the present invention just is to provide a kind of oil-soluble stamp-pad ink/ink paste seal literary composition method of formation time relatively of identifying.
The object of the present invention is achieved like this: a kind of oil-soluble stamp-pad ink/ink paste seal literary composition method of formation time relatively of identifying, it is characterized in that: it is by difference replicate determination seal literary composition to be checked and the civilian dissolution rate of reference sample seal, then it is compared, thereby judge the civilian relative formation time of seal to be checked.
The above-mentioned evaluation oil-soluble stamp-pad ink/ink paste seal literary composition method of formation time relatively is to carry out as follows: a), whether the impress check that forms check, the civilian carrier paper of seal to be checked and the check of seal to be checked literary composition used oil dissolubility stamp-pad ink or ink paste kind of oil-soluble stamp-pad ink or ink paste of seal literary composition to be checked and the check of carrier preservation condition thereof, seal literary composition to be checked; B), from the sample storehouse, filter out reference sample seal literary composition; C), difference replicate determination seal literary composition to be checked and the civilian dissolution rate of reference sample seal, then the dissolution rate that prints civilian dissolution rate and reference sample seal literary composition to be checked is compared and judges civilian priority or the degree of closeness of printing civilian formation time with respect to the reference sample of printing to be checked: the dissolution rate as if seal literary composition to be checked prints civilian dissolution rate less than the reference sample, and the formation time of literary composition of printing then to be checked is early than the civilian formation time of reference sample seal; If the dissolution rate of seal literary composition to be checked is greater than the dissolution rate of reference sample seal literary composition, the formation time of seal literary composition then to be checked is later than the formation time of reference sample seal literary composition; If the dissolution rate of seal literary composition to be checked prints the dissolution rate of literary composition more near the reference sample, the formation time of seal literary composition then to be checked is more near the civilian formation time of reference sample seal.
Above-mentioned seal literary composition to be checked and carrier preservation condition thereof verify as range estimation or/and microexamination, is determined whether the civilian carrier of seal to be checked exists or/and alternative light source check and scraped, disappears and the unusual vestige of preserving such as take off.For the Yin Wen of normal preservation, oil-soluble stamp-pad ink or ink paste are impressed and are formed check to carry out next step seal literary composition to be checked.
Above-mentioned seal literary composition to be checked whether oil-soluble stamp-pad ink or ink paste impress that to form check be by the ester class or/and a small amount of seal literary composition of alcohol organic solvent dissolving to observe its solubility property, preferably with the lower member ester class or/and alcohol organic solvent is extracted a small amount of seal literary composition on the normal seal literary composition to be checked of above-mentioned preservation, the difficulty or ease of observing solubility property are to determine whether the formation of impressing of oil-soluble stamp-pad ink or ink paste, can dissolving be the formation of impressing of oil-soluble stamp-pad ink or ink paste, carry out the civilian carrier paper examination of next step seal to be checked.
The civilian carrier paper of above-mentioned seal to be checked verify as range estimation or/and microexamination or/and thickness measurement or/and the check of paper fibre and paper pulp kind.
Above-mentioned seal to be checked civilian used oil dissolubility stamp-pad ink or ink paste print that verifying as of civilian kind measured its infrared spectrum or/and Raman spectrum or/and fluorescence spectrum, and carries out thin-layer chromatographic analysis to the civilian colorant of seal to be checked.
With seal stationery to be checked comparability is arranged in order to ensure reference sample seal literary composition, the above-mentioned reference sample seal literary composition that filters out from the sample storehouse is to filter out the sample seal literary composition consistent with the civilian described Interventions Requested result of seal to be checked as reference sample seal literary composition from the sample storehouse.(each Interventions Requested is clear and definite in the sample storehouse).
Can guarantee the consistance of the stamp-pad ink of seal literary composition to be checked and reference seal literary composition or ink paste composition, paper condition, preservation condition by above step, be to carry out the mensuration of next step dissolution rate and the basis of comparison.
Above-mentioned replicate determination respectively seal literary composition to be checked carries out according to the following steps with the dissolution rate of reference sample seal literary composition: at a certain temperature, cut the deep or light uniform seal literary composition to be checked of color and luster at first respectively and print the part impression of civilian equal area size with the reference sample; After dissolving respectively with the equivalent organic solvent then, sample from civilian the printing the civilian lysate of seal to be checked simultaneously respectively with the reference sample in a plurality of time points; The civilian meltage of seal in each sampling of replicate determination respectively at last, and calculate above-mentioned seal literary composition to be checked and the civilian dissolution rate of reference sample seal respectively by the meltage/final meltage of dissolution rate=sometime.
Refer to 16～20 ℃ under the above-mentioned uniform temperature; Above-mentioned organic solvent is alcohols and ester class binary system, and its proportioning is an alcohols: ester class=1～2: 1; Above-mentioned a plurality of time point refers to 2～5 time points, and the 1st time point and last time point should be separated by more than 2 hours; The civilian meltage of seal is to adopt thin-layered chromatography (TLC) or high performance liquid chromatography (HPLC) or ultravioletvisible spectroscopy (UV-Vis) to carry out quantitative test in each sampling of above-mentioned replicate determination respectively; Above-mentioned final meltage is the meltage in last time point sampling.
Above-mentioned alcohols particular methanol or ethanol or butanols or amylalcohol, above-mentioned ester class ethyl acetate or butyl acetate, its proportioning is an alcohols: ester class=1～2: 1.
When printing civilian meltage in adopting each sampling of thin-layered chromatography difference replicate determination, its analysis condition is: adsorbent is silica gel H SG F
254, the volume ratio of normal butyl alcohol, ethanol, water, glacial acetic acid is followed successively by in the developping agent: 9: 1: 1: 1, launch 16～20 ℃ of temperature, duration of run 10min～20min; When adopting thin layer chromatogram scanner to scan, the detection wavelength is 510nm.
When printing civilian meltage in adopting each sampling of high performance liquid chromatography difference replicate determination, its analysis condition is: chromatographic column: 5 μ m C18 posts, moving phase: methyl alcohol/acetonitrile 90: 10, flow velocity: 0.5mL/min, ultraviolet detection wavelength: 254nm.
When printing civilian meltage in adopting each sampling of ultravioletvisible spectroscopy difference replicate determination, its analysis condition is: measure wavelength 510nm.
Check by seal literary composition to be checked being carried out strict preservation condition among the present invention, the impress steps such as check that form check, carrier paper examination, used common ink paste or stamp-pad ink kind of oil-soluble stamp-pad ink or ink paste can guarantee the reference sample seal literary composition and the civilian consistance on preservation condition, carrier (paper), ink paste or stamp-pad ink kind of seal to be checked that filter out, guaranteeing that the reference sample seal literary composition that filters out has comparability with seal stationery to be checked, is to carry out the mensuration of next step dissolution rate and the basis of comparison; By the civilian dissolution rate of seal literary composition to be checked and reference sample seal is carried out replicate determination and comparison, judge that seal literary composition to be checked prints the priority or the degree of closeness of civilian formation time with respect to the reference sample then.Under consistent situation such as preservation condition, carrier (paper), ink paste or stamp-pad ink kind, the relative smaller of dissolution rate, degree of aging is higher relatively, and it is remote relatively to print civilian formation time.That is to say, the dissolution rate of dissolution rate that seal to be checked is civilian and reference sample seal literary composition compares judges literary composition prints civilian formation time with respect to the reference sample priority or the degree of closeness of printing to be checked: if the dissolution rate of literary composition that prints to be checked is significantly less than the civilian dissolution rate of reference sample seal, the degree of aging of seal literary composition then to be checked is higher relatively, and its formation time is obviously early than the civilian formation time of reference sample seal; If the dissolution rate of seal literary composition to be checked is significantly greater than the dissolution rate of reference sample seal literary composition, the degree of aging of seal literary composition then to be checked is relatively low, and its formation time is later than the formation time of reference sample seal literary composition certainly; If the dissolution rate of seal literary composition to be checked prints the dissolution rate of literary composition more near the reference sample, the formation time of seal literary composition then to be checked is more near the civilian formation time of reference sample seal.
Result of the present invention accurately and reliably, simple to operate, be easy to promote, can be widely used in the impress relative formation time of the seal literary composition that forms of oil-soluble stamp-pad ink or ink paste and identify.Adopt the present invention can determine under having in 3 terms that oil-soluble stamp-pad ink or ink paste are impressed and form the relative formation time of seal literary composition with this situation of kind reference.
Embodiment
Further specify the present invention below by embodiment, but the present invention is not limited to these embodiment.
Embodiment 1: the seal literary composition of choosing the red ink paste/oil cap impression one-tenth that is formed at " January calendar year 2001 " is seal literary composition to be checked.
A kind of oil-soluble stamp-pad ink/ink paste seal literary composition method of formation time relatively of identifying, it is characterized in that: it is to carry out as follows:
(1) check of seal literary composition to be checked and carrier preservation condition thereof: by range estimation, microexamination and alternative light source check, determining whether seal literary composition to be checked and carrier thereof exist scrapes, disappears and the unusual vestige of preserving such as take off, for preserving normal sample seal literary composition, following step check.
(2) seal literary composition to be checked whether oil-soluble stamp-pad ink or ink paste impress and form check: with a small amount of seal literary composition on ethyl acetate or the civilian carrier of methanol extraction seal to be checked, whether the difficulty or ease of observation solubility property judge the formation of impressing of oil-soluble stamp-pad ink or ink paste.Under this solvent action, what can dissolve is oil-soluble stamp-pad ink or ink paste, and undissolvable is water-soluble stamp-pad ink, the special stamp-pad ink of atom seal wet goods.Judge the sample seal literary composition that can dissolve, following step check.
(3) the civilian carrier paper examination of seal to be checked: to the civilian carrier paper of seal to be checked estimate, microexamination, thickness measurement, paper fibre and the check of paper pulp kind.
(4) check of seal to be checked civilian used oil dissolubility stamp-pad ink or ink paste kind: measure the civilian infrared spectrum of seal to be checked, Raman spectrum and fluorescence spectrum; The civilian colorant of seal to be checked is carried out thin-layer chromatographic analysis.Reddish oil dissolubility stamp-pad ink or ink paste colorant have two kinds of situations usually through thin-layer chromatographic analysis after the expansion: a kind of is that orange, red two color spots are arranged from bottom to up; A kind of is to have only red grouper.Can determine the colorant composition of seal to be checked civilian used oil dissolubility stamp-pad ink or ink paste according to color spot number, color, position.
(5) screening reference sample seal literary composition: sample seal literary composition is carried out the above-mentioned project check identical with seal literary composition to be checked, and therefrom filter out the above-mentioned project assay sample seal literary composition consistent as reference sample seal literary composition 1 (formation time 2001.3), reference sample seal literary composition 2 (formation times 2004.3) with seal literary composition to be checked.
Can guarantee to treat that by above step sample seal literary composition and reference sample print the consistance of civilian preservation condition, carrier paper, ink paste or stamp-pad ink kind, be the basis of further checking.
(6) difference replicate determination seal literary composition to be checked and the civilian dissolution rate of reference sample seal:
A, cut equal area (8～10mm respectively
2), the part impression of the deep or light uniform seal literary composition to be checked of color and luster, reference sample seal literary composition, be cut into 1mm
2Segment to be analyzed.
20 ℃ of b, temperature, ethyl acetate and above-mentioned each the impression sample of normal butyl alcohol binary solvent (volume ratio 1: 1) dissolving with equivalent, and extracting above-mentioned each impression respectively at 40s, 2min, 6min and each time point more than the 120min, each extract of gained is to be analyzed.
C, employing thin-layered chromatography (TLC) are printed civilian meltage in above-mentioned each extract of replicate determination respectively: its analysis condition is: adsorbent is silica gel H SG F
254, the volume ratio of normal butyl alcohol, ethanol, water, glacial acetic acid is followed successively by in the developping agent: 9: 1: 1: 1, launch 20 ℃ of temperature, duration of run 10min.Adopt thin layer chromatogram scanner to scan, the detection wavelength is 510nm.The integral area (being meltage) of record chromatographic peak.Experimental data such as table 1:
Table 1: seal literary composition to be checked, reference sample print civilian different time points meltage
Annotate: meltage is characterized by TLC scanner scanning gained chromatographic peak area integrated value, no unit.
(7) determine seal literary composition to be checked formation time relatively:
Calculate the dissolution rate that seal literary composition to be checked, reference sample print civilian different time points (dissolution rate=sometime meltage/final meltage) respectively, wherein dissolution time is that the seal to be checked measured more than 2 hours is civilian, to print civilian meltage be final meltage to the reference sample.The dissolution rate that is calculated by table 1 sees Table 2.
Table 2: the dissolution rate that calculates by table 1
At the parallel comparative result that records dissolution rate of each time point, judges civilian priority or the degree of closeness of printing civilian formation time with respect to the reference sample of printing to be checked according to above-mentioned seal to be checked literary composition and reference sample seal literary composition.Under the situation of preservation condition, carrier (paper), ink paste or stamp-pad ink kind unanimity, the relative smaller of dissolution rate, degree of aging is higher relatively, and it is remote relatively to print civilian formation time.In the above-mentioned table 2 initial each the time point dissolution rate of seal literary composition to be checked be significantly less than formation time be 2004.3 sample seal literary composition and with formation time be that 2001.3 sample seal literary composition is approaching, illustrate that civilian degree of aging of seal to be checked and formation time are that 2001.3 sample seal literary composition is approaching, so both formation times are approaching.
Embodiment 2: the seal literary composition of choosing the orange ink paste/oil cap impression one-tenth that is formed at " in November, 2006 " is seal literary composition to be checked.
A kind of oil-soluble stamp-pad ink/ink paste seal literary composition method of formation time relatively of identifying, it is characterized in that: it is to carry out as follows:
(1) check of the civilian preservation condition of seal to be checked:, determine whether seal literary composition to be checked exists to scrape, disappear and the unusual vestige of preserving such as take off that for preserving normal sample seal literary composition, the following step will be checked by range estimation, microexamination and alternative light source check.
(2) seal literary composition to be checked whether oil-soluble stamp-pad ink or ink paste impress and form check: with a small amount of seal literary composition on ethyl acetate and the civilian carrier of alcohol extract seal to be checked, whether the difficulty or ease of observation solubility property judge the formation of impressing of oil-soluble stamp-pad ink or ink paste.Under this solvent action, what can dissolve is oil-soluble stamp-pad ink or ink paste, and undissolvable is water-soluble stamp-pad ink, the special stamp-pad ink of atom seal wet goods.Judge the sample seal literary composition that can dissolve, following step check.
(3) the civilian carrier paper examination of seal to be checked: to the civilian carrier paper of seal to be checked estimate, microexamination, thickness measurement, paper fibre and the check of paper pulp kind.
(4) check of seal to be checked civilian used oil dissolubility stamp-pad ink or ink paste kind: measure the civilian infrared spectrum of seal to be checked, Raman spectrum and fluorescence spectrum; The civilian colorant of seal to be checked is carried out thin-layer chromatographic analysis.Orange oil dissolubility stamp-pad ink or ink paste colorant have two kinds of situations usually through thin-layer chromatographic analysis after the expansion: a kind of is that orange, red two color spots are arranged from bottom to up; A kind of is to have only orange spot.Can determine the colorant composition of seal to be checked civilian used oil dissolubility stamp-pad ink or ink paste according to color spot number, color, position.
(5) screening reference sample seal literary composition: sample seal literary composition is carried out the above-mentioned project check identical with seal literary composition to be checked, and therefrom filter out the above-mentioned project assay sample seal literary composition consistent as reference sample seal literary composition 1 (formation time 2005.11), reference sample seal literary composition 2 (formation times 2006.11) with seal literary composition to be checked.
Can guarantee to treat that by above step sample seal literary composition and reference sample print the consistance of civilian preservation condition, carrier paper, ink paste or stamp-pad ink kind, be the basis of further checking.
(6) difference replicate determination seal literary composition to be checked and the civilian dissolution rate of reference sample seal:
A, cut equal area (8～10mm respectively
2), the part impression of the deep or light uniform seal literary composition to be checked of color and luster, reference sample seal literary composition, be cut into 1mm
2Small pieces to be analyzed;
18 ℃ of b, temperature are used the butyl acetate of equivalent and ethanol binary solvent (volume ratio 2: 3) to dissolve above-mentioned each impression sample, and are extracted above-mentioned each impression respectively at 30s, 90s, 5min and each time point more than the 120min, and each extract of gained is to be analyzed;
C, employing thin-layered chromatography (TLC) are printed civilian meltage in above-mentioned each extract of replicate determination respectively: its analysis condition is: adsorbent is silica gel H SG F
254, the volume ratio of normal butyl alcohol, ethanol, water, glacial acetic acid is followed successively by in the developping agent: 9: 1: 1: 1, launch 18 ℃ of temperature, duration of run 15min.Adopt thin layer chromatogram scanner to scan, the detection wavelength is 510nm.The integral area (being meltage) of record chromatographic peak.Experimental data such as table 3.
Table 3: seal literary composition to be checked, reference sample print civilian different time points meltage
Annotate: meltage is a TLC scanner scanning gained chromatographic peak area integrated value, no unit.
(7) determine seal literary composition to be checked formation time relatively:
Calculate the dissolution rate that seal literary composition to be checked, reference sample print civilian different time points (dissolution rate=sometime meltage/final meltage) respectively, wherein dissolution time is that the seal to be checked measured more than 2 hours is civilian, to print civilian meltage be final meltage to the reference sample.The dissolution rate that is calculated by table 3 sees Table 4.
Table 4: the dissolution rate that calculates by table 3
At the parallel comparative result that records dissolution rate of each time point, judges civilian priority or the degree of closeness of printing civilian formation time with respect to the reference sample of printing to be checked according to above-mentioned seal to be checked literary composition and reference sample seal literary composition.Under the situation of preservation condition, carrier (paper), ink paste or stamp-pad ink kind unanimity, the relative smaller of dissolution rate, degree of aging is higher relatively, and it is remote relatively to print civilian formation time.Initial each the time point dissolution rate of above-mentioned seal literary composition to be checked is obviously approaching with 2006.11 reference samples seal literary composition 2 greater than 2005.11 reference samples seal literary composition 1, civilian degree of aging of seal then to be checked and 2006.11 reference samples seal literary composition 2 are approaching, so the formation time of seal literary composition to be checked and 2006.11 reference samples seal literary composition 2 are approaching, be to form for 2006.11 same periods.
Embodiment 3: seal literary composition to be checked is rose ink paste/oil cap impression Cheng Yinwen.
In its authentication step, when replicate determination seal literary composition to be checked prints the dissolution rate of literary composition with the reference sample, ethyl acetate and methyl alcohol binary solvent (volume ratio 2: 3) with equivalent dissolve its seal literary composition to be checked, reference sample seal literary composition, respectively at 1min, 3min, 10min, each above time point of 30min and 180min prints the civilian lysate and samples from seal literary composition to be checked, reference sample simultaneously, measures its meltage then respectively.
Meltage is measured and is adopted ultravioletvisible spectroscopy (UV-Vis) quantitative test, measures the absorbance under the 510nm.
All the other steps are with embodiment 1.
Embodiment 4: seal literary composition to be checked is red ink paste/oil cap impression Cheng Yinwen.
In its authentication step, when replicate determination seal literary composition to be checked prints the dissolution rate of literary composition with the reference sample, butyl acetate and amylalcohol binary solvent (volume ratio 2: 3) with equivalent dissolve its seal literary composition to be checked, reference sample seal literary composition, print the civilian lysate and sample from seal literary composition to be checked, reference sample simultaneously respectively at 2min, 5min, 15min and each time point more than the 180min, measure its meltage then respectively.
Meltage is measured and is adopted high performance liquid chromatography (HPLC), and its analysis condition is: chromatographic column: 5 μ m C18 posts, moving phase: methyl alcohol/acetonitrile 90: 10, flow velocity: 0.5mL/min, ultraviolet detection wavelength: 254nm.
All the other steps are with embodiment 1.
Claims (10)
1, a kind of oil-soluble stamp-pad ink/ink paste seal literary composition method of formation time relatively of identifying, it is characterized in that: it is by difference replicate determination seal literary composition to be checked and the civilian dissolution rate of reference sample seal, then it is compared, thereby judge the civilian relative formation time of seal to be checked.
2, the evaluation oil-soluble stamp-pad ink as claimed in claim 1/ink paste seal literary composition method of formation time relatively, it is characterized in that: it is to carry out as follows: a), whether the impress check that forms check, the civilian carrier paper of seal to be checked and the check of seal to be checked literary composition used oil dissolubility stamp-pad ink or ink paste kind of oil-soluble stamp-pad ink or ink paste of seal literary composition to be checked and the check of carrier preservation condition thereof, seal literary composition to be checked; B), from the sample storehouse, filter out reference sample seal literary composition; C), difference replicate determination seal literary composition to be checked and the civilian dissolution rate of reference sample seal, then the dissolution rate that prints civilian dissolution rate and reference sample seal literary composition to be checked is compared and judges civilian priority or the degree of closeness of printing civilian formation time with respect to the reference sample of printing to be checked: the dissolution rate as if seal literary composition to be checked prints civilian dissolution rate less than the reference sample, and the formation time of literary composition of printing then to be checked is early than the civilian formation time of reference sample seal; If the dissolution rate of seal literary composition to be checked is greater than the dissolution rate of reference sample seal literary composition, the formation time of seal literary composition then to be checked is later than the formation time of reference sample seal literary composition; If the dissolution rate of seal literary composition to be checked prints the dissolution rate of literary composition more near the reference sample, the formation time of seal literary composition then to be checked is more near the civilian formation time of reference sample seal.
3, the evaluation oil-soluble stamp-pad ink as claimed in claim 2/ink paste seal literary composition method of formation time relatively is characterized in that: described seal literary composition to be checked and carrier preservation condition thereof verify as range estimation or/and microexamination or/and the alternative light source check; Impress described seal literary composition to be checked to form check be by the ester class or/and a small amount of seal literary composition of alcohol organic solvent dissolving is judged to observe its solubility property by oil-soluble stamp-pad ink or ink paste; The civilian carrier paper of described seal to be checked verify as range estimation or/and microexamination or/and thickness measurement or/and the check of paper fibre and paper pulp kind; The verifying as of described seal to be checked civilian used oil dissolubility stamp-pad ink or ink paste kind measures its infrared spectrum or/and Raman spectrum or/and fluorescence spectrum, and carries out thin-layer chromatographic analysis to the civilian colorant of seal to be checked.
4, the civilian method of formation time relatively of evaluation oil-soluble stamp-pad ink as claimed in claim 2/ink paste seal is characterized in that: the described reference sample seal literary composition that filters out from the sample storehouse is to filter out the sample seal literary composition consistent with the civilian described Interventions Requested result of seal to be checked to print literary composition as the reference sample from the sample storehouse.
5, the method for evaluation oil-soluble stamp-pad ink as claimed in claim 1/relative formation time of ink paste seal literary composition, it is characterized in that: described replicate determination respectively seal literary composition to be checked carries out according to the following steps with the dissolution rate of reference sample seal literary composition: at a certain temperature, cut the deep or light uniform seal literary composition to be checked of color and luster at first respectively and print the part impression of civilian equal area size with the reference sample; After dissolving respectively with the equivalent organic solvent then, sample from civilian the printing the civilian lysate of seal to be checked simultaneously respectively with the reference sample in a plurality of time points; The civilian meltage of seal in each sampling of replicate determination respectively at last, and calculate described seal literary composition to be checked and the civilian dissolution rate of reference sample seal respectively by the meltage/final meltage of dissolution rate=sometime.
6, the method for evaluation oil-soluble stamp-pad ink as claimed in claim 5/relative formation time of ink paste seal literary composition is characterized in that: refer to 16～20 ℃ under the described uniform temperature; Described organic solvent is alcohols and ester class binary system; Described a plurality of time point refers to 2～5 time points, and the 1st time point and last time point should be separated by more than 2 hours; The civilian meltage of seal is to adopt thin-layered chromatography or high performance liquid chromatography or ultravioletvisible spectroscopy to carry out quantitative test in each sampling of described replicate determination respectively; Described final meltage is the meltage in last time point sampling.
7, the method for evaluation oil-soluble stamp-pad ink as claimed in claim 6/relative formation time of ink paste seal literary composition, it is characterized in that: described alcohols is methyl alcohol or ethanol or butanols or amylalcohol, described ester class is ethyl acetate or butyl acetate, and the proportioning of described alcohols and ester class binary system is an alcohols: ester class=1～2: 1.
8, the method for evaluation oil-soluble stamp-pad ink as claimed in claim 6/relative formation time of ink paste seal literary composition, it is characterized in that: the civilian meltage of seal is that its analysis condition is: adsorbent is silica gel H SG F when adopting thin-layered chromatography to carry out quantitative test in each sampling of described replicate determination respectively
254, developping agent: the volume ratio of normal butyl alcohol, ethanol, water, glacial acetic acid is followed successively by: 9: 1: 1: 1, launch 16～20 ℃ of temperature, duration of run 10～20min; When adopting thin layer chromatogram scanner to scan, the detection wavelength is 510nm.
9, the method for evaluation oil-soluble stamp-pad ink as claimed in claim 6/relative formation time of ink paste seal literary composition, it is characterized in that: the civilian meltage of seal is when adopting high performance liquid chromatography to carry out quantitative test in each sampling of described replicate determination respectively, its analysis condition is: chromatographic column: 5 μ m C18 posts, moving phase: methyl alcohol/acetonitrile 90: 10, flow velocity: 0.5mL/min, ultraviolet detection wavelength: 254nm.
10, the method for evaluation oil-soluble stamp-pad ink as claimed in claim 6/relative formation time of ink paste seal literary composition, it is characterized in that: the civilian meltage of seal is that its analysis condition is: measure wavelength 510nm when adopting ultravioletvisible spectroscopy to carry out quantitative test in each sampling of described replicate determination respectively.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101975758A (en) * | 2010-09-17 | 2011-02-16 | 刘公民 | Method for authenticating relative writing time of contract or written pledge |
| CN103105385A (en) * | 2013-01-29 | 2013-05-15 | 沈阳博兴亚达科技有限公司 | Method for spectral fluorescence detection and three-dimensional rotating microscope testing of sequence of crossed writings and seal stamps |
| CN105044069A (en) * | 2015-08-12 | 2015-11-11 | 合肥源信智能仪器有限公司 | Laser fluorescence inspection method for recognizing sequence of crossed writing and seal stamp |
| CN107037030A (en) * | 2017-04-01 | 2017-08-11 | 王艳 | Printed text and the red and black sequential authentication method under writing not crossing instances |
| CN109187371A (en) * | 2018-09-04 | 2019-01-11 | 辽宁警察学院 | The method of red and black timing is judged based on YIQ color mode |
-
2007
- 2007-05-22 CN CN 200710078489 patent/CN101059497A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101975758A (en) * | 2010-09-17 | 2011-02-16 | 刘公民 | Method for authenticating relative writing time of contract or written pledge |
| CN103105385A (en) * | 2013-01-29 | 2013-05-15 | 沈阳博兴亚达科技有限公司 | Method for spectral fluorescence detection and three-dimensional rotating microscope testing of sequence of crossed writings and seal stamps |
| CN105044069A (en) * | 2015-08-12 | 2015-11-11 | 合肥源信智能仪器有限公司 | Laser fluorescence inspection method for recognizing sequence of crossed writing and seal stamp |
| CN107037030A (en) * | 2017-04-01 | 2017-08-11 | 王艳 | Printed text and the red and black sequential authentication method under writing not crossing instances |
| CN109187371A (en) * | 2018-09-04 | 2019-01-11 | 辽宁警察学院 | The method of red and black timing is judged based on YIQ color mode |
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