CN102818823B - Method for detecting writing time of carbon-containing ink handwriting by measuring electrical conductivity of stroke - Google Patents
Method for detecting writing time of carbon-containing ink handwriting by measuring electrical conductivity of stroke Download PDFInfo
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- CN102818823B CN102818823B CN201210274504.3A CN201210274504A CN102818823B CN 102818823 B CN102818823 B CN 102818823B CN 201210274504 A CN201210274504 A CN 201210274504A CN 102818823 B CN102818823 B CN 102818823B
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Abstract
The invention relates to a method for detecting the writing time of a carbon-containing ink handwriting by measuring the electrical conductivity of a stroke. The detailed method comprises the following steps of: arranging a stoke to be measured in a sealed humiture environment, measuring out the electrical conductivity value of the stoke to be measured in the current environment by using an electrical conductivity measuring apparatus after the electrical conductivity of the stoke is stable; then changing the temperature or humidity of the sealed environment to change the electrical conductivity value of the stroke to be measured, and meanwhile, recording the variation rate of the electrical conductivity value of the stroke to be measured within a certain time, and drawing an electrical conductivity curve graph corresponding to the time; determining that the stroke to be measured is formed in recent time if the variation amplitude of the electrical conductivity curve is large, and determining that the stroke to be measured is formed before if the variation of the electrical conductivity curve is small. The writing time of the carbon-containing ink handwriting is initiated through the method which is simple and easy to implement, can be used for detecting and analyzing only according to the stroke of the handwriting without using a comparison sample, so that the method is an absolute time detection method and can be used as the basis of forensic authentication.
Description
[technical field]
The present invention relates to a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time.
[background technology]
Write formation time check and can be divided into the Relative writing age check of file and the absolute formation time check of file.So-called relative time check, refers to the check of comparison sample, by sample and sample are compared, the formation time of determining sample be the elder generation of sample or after; So-called absolute time check is directly sample to be carried out to time check, does not need to compare sample.
The relative time that is mostly that China can carry out is at present checked.The check of first colorant composition.As long as the sample file with sample file same ink, identical paper, identical preservation condition can be provided, utilizing the priority of mass spectrometer, various spectrometer and some physics, chemical method authenticating document formation time is not a difficult problem, but often cannot find qualified sample file in actual inspection case, unless the sample of confession comparison inspection and sample are for to write on same a piece of paper with one-pen.As compare sample and can not meet above-mentioned condition, which kind of comparison method to be all unscientific with in theory.It two is interim comparison inspections.Comprise the differentiation of paper and print characteristics, variation characteristic of seal impression etc.Such as atom print, because it prints plane materiel matter, be expanded rubber, first easy to wear; The comparison sample that provides more comprehensive different times to impress has interim oiling feature, if can judge that sample printed text and sample printed text when approach again.Dipping in printed text that ink paste impresses and sometimes have a stain certain special time period is included, is also the important evidence of comparison inspection.
The method of inspection of the absolute formation time of file has sulfate diffusion method, stamped method, extraction, dissolution with solvents method, volatile ingredient determination method etc., but because of word colorant, preservation condition ever-changing, with kind ink, with the time, write but originate different files often experimental data difference go against accepted conventions, therefore above method can not be as appraisal basis.In a word, for the check of writing formation time, except a few method of formally identifying by project verification, most methods of inspection are all laboratory methods, are the static check methods of setting up in the ideal situation.
Carbon containing ink writing, being often referred to carbon steel board pen ink writing or carbon content is main gel pen ink writing.The method of formation time write in check writing in the field of judicial expertise at present, is mainly all stroke, the seal impression for organic toner composition, as ball pen, color inks, ink paste stamp-pad ink etc.But for burnt black ink, carbon containing gel pen ink, because its principal ingredient carbon element can not be extracted for instrumental analysis by any organic solvent, according to current report, all can not write formation time to it both at home and abroad and test.But the main writing implement using in people's daily life is at present signature pen, and its ink composition major part is carbon containing ink, so in the urgent need to the method for inspection of carbon containing ink writing writing time.
[summary of the invention]
The present invention is for overcoming the deficiencies in the prior art part, provide a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time, the method only, according to the analysis of just testing of sample writing stroke itself, does not need to compare sample, is a kind of absolute time method of inspection.
The technical scheme that technical solution problem of the present invention adopts is: a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time, comprise the following steps:
Stroke to be checked is positioned in airtight humiture environment, after its stable conductivity, with conductivity measurement device measuring, goes out the electric conductivity numerical value of this stroke to be checked in current environment; Then change temperature or the humidity of this closed environment, the electric conductivity numerical value of this stroke to be checked is changed, record within a certain period of time the rate of change of the electric conductivity numerical value of this stroke to be checked, and draw its electric conductivity curve map corresponding with the time simultaneously; If this electric conductivity curvilinear motion amplitude is larger, judge that this stroke to be checked is to write in the recent period formation; If it is less that electric conductivity changes, judge that sample stroke is to write formation long term.
As the further improvement of such scheme, described conductivity measurement equipment is high resistant instrument, conductivity meter or micro current instrument.
As the further improvement of such scheme, the range of humidity variation of described closed environment is 0.01%～100%RH.
As the further improvement of such scheme, the range of temperature of described closed environment is 10 ℃～40 ℃.
As the further improvement of such scheme, described closed environment is closed container or humiture environmental test chamber.
Inventive principle:
The carbon containing ink stroke of writing more remote, in the variation repeatedly of having experienced natural temperature, humidity, paper do again and again shrink, stretching exercise, carbon granule has penetrated into paper fibre inside, has more stably been combined with fiber, thus at paper, be dried, humidification causes paper fibril aggregation or while stretching resistance change less; And the stroke carbon granule of more recently writing not yet experiences natural temperature, humidity changes, more float over paper surface, when paper humidification, because paper makes moist to uphold, cause the carbon granule spacing being attached on fiber to increase, thereby cause that larger variation occurs resistance value.Therefore,, when changing the external conditions such as temperature humidity, can correspondingly there is larger variation in the resistance value of carbon containing stroke.More remote writing is subject to external condition variable effect less as the stroke before a year, recently the stroke as nearly a week of writing is subject to impact that external condition changes greatly, we are the unit interval resistance change rate size when changing external condition according to stroke, just can determine the actual writing time of sample stroke.
The beneficial effect of this method has been to start the new approaches of check carbon containing ink writing writing time, the method is simple and easy to realize, and only, according to the analysis of just testing of sample writing stroke itself, does not need to compare sample, be a kind of absolute time method of inspection, can be used as the foundation of judicial expertise.
[accompanying drawing explanation]
The invention will be further described in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is experimental provision schematic diagram of the present invention,
Fig. 2 is the electric conductivity curve map of embodiment 1,
Fig. 3 is the electric conductivity curve map of embodiment 2,
Fig. 4 is the electric conductivity curve map of embodiment 3.
In figure: 1, closed container; 2, freeze-day with constant temperature gas interface; 3, constant temperature and humidity gas interface; 4, objective table; 5, potential electrode; 6, stroke; 7, conductivity measurement device; 8, computing machine
[embodiment]
Experimental provision of the present invention forms as shown in Figure 1, and the concrete method of inspection is carried out as follows:
1, choose stroke: the carbon containing ink writing stroke that selection length is 2cm-5cm is as stroke 6 to be checked.As inadequate in stroke length, while being less than the stroke section of 2cm for several, can adopt with the stronger HB of electric conductivity or Pencil with 2B hardness several adjacent short stroke sections are connected into the long stroke segmented mode that meets above-mentioned length (can not be straight line), form the circuit with graphite line (being considered as wire) series connection carbon element stroke (being considered as resistance).At the two ends of stroke (or circuit), with pencil contact pen, draw a picture out graphite linings that diameter is greater than 2mm as electrode 5, to increase the contact area of measurement mechanism metal electrode and stroke, prevent loose contact.
2, image data: described stroke to be checked is positioned on the objective table 4 in closed container 1 (or humiture environmental test chamber), closed container 1 has two interfaces, one of them interface 2 connects freeze-day with constant temperature gas source of the gas, another interface 3 connects constant temperature and humidity gas source of the gas, and the temperature of setting in this closed container is 30 ℃.Conductivity measurement equipment 7 (is used to high resistant instrument, conductivity meter or micro current instrument, following high resistant instrument represents conductivity measurement equipment) two potential electrode be closely pressed in respectively in the two end electrodes 5 of stroke circuit, the data-out port of conductivity measurement equipment 7 connects computing machine 8.By interface 2, to closed container 1, continuing to pass into temperature is that the High Purity Nitrogen gas of 30 ℃ is dried, and in the time of the 10th minute, (humidity is 0.01%RH) its stable conductivity, starts to continue to record resistance data 100 seconds.Then by interface 3, to closed container 1, passing into temperature is the water vapor that 30 ℃, humidity are 100%RH, starts when importing water vapor to carry out the dynamic acquisition resistance data line item of going forward side by side every 2 Miao Weiyige chronomeres, in the time of the 100th second, stops.
3, detect data: the sample stroke resistance value measuring after passing into saturated steam, within the unit interval, significant change can occur, no matter numerical value becomes large or diminishes, and gets its absolute value.With the resistance value R2 of next chronomere, the resistance value R1 of Jian Shangyige chronomere, except the above Yi Ge resistance value R1 of chronomere, is defined as resistance change rate Δ R.First 2 seconds is Δ R1, and second 2 seconds is Δ R2 ... drawing out horizontal ordinate is that detection time, ordinate are the curve map of Δ R.When meeting discovery Δ R is a beginning, then very brief rising sharply declines and with detection time, extends the curve tending to be steady gradually.
4, experimental analysis:
4.1, for same one-pen, once write together the carbon containing ink stroke on same a piece of paper, no matter be cut-off line, curve 2cm or 5cm, the time curve of its Δ R is basic identical, illustrate that this method of inspection is to the carbon containing ink stroke under same book write condition, the sample length size of stroke or mode are little on testing result impact.
4.2, more several different carbon containing ink stroke Δ R features: experimental subjects is for writing the year before on same a piece of paper but the different carbon containing ink stroke of brand, the resistance change curve of every kind of stroke has different, but difference is little, as the stroke of different inks pass into saturated steam after Δ R1 be generally less than 4%, Δ R2 is generally less than 2%.
4.3, for same one-pen is same, once write the carbon containing ink stroke on different paper, the time curve of its Δ R has certain variation, be similar to upper and lower global displacement, but tracing pattern is basic identical.For example the Δ R1 on A paper is 4%, and the Δ R1 on B paper is 4.3%, and the Δ R1 on C paper is 3.8%, and different paper factor is little on testing result impact.
4.4, for same one-pen the year before before (long term) and one week (in the recent period) write the carbon containing ink stroke on same a piece of paper, it is the impact on Δ R of the writing time of our primary study, find when stroke resistance before one week is initial to change greatly, then sharply reduce, as after passing into saturated steam, first 2 seconds Δ R1 change over 5%; Second 2 seconds Δ R2 changes over 4.5%.And that stroke resistance the year before changes when initial is milder, as passes into after saturated steam first 2 seconds Δ R1 and change and be less than 2%, the second 2 seconds Δ R2 and be less than 1.8%.Both are at the form of Δ R time curve: the Δ R time curve descending slope of stroke is very large in the recent period, and the Δ R time curve descending slope of stroke at a specified future date is milder.
5, the method for inspection of carbon containing ink writing writing time:
5.1, single measurement method: the formation time of writing of determining sample stroke according to the rate of change of Δ R.
From above-mentioned experiment, learn, the person's handwriting of writing for (the year before) at a specified future date, no matter be the sample length of stroke, different paper, the carbon containing ink of heterogeneity, it is less from dry environment Δ R fall when adding wet environment, if Δ R1 is 2%, Δ R2 is 1.8%, and Δ R3 is 1.77%, Δ R4 is 1.76%, and Δ R5 is 1.75% ...To the person's handwriting that write (in a week) in the near future, no matter be the sample length of stroke, different paper, the carbon containing ink of heterogeneity, it declines by a big margin from dry environment Δ R when adding wet environment, if Δ R1 is 5%, Δ R2 is 3.5%, Δ R3 is 3%, and Δ R4 is 2.6%, and Δ R5 is 2.3% ...This phenomenon checks the formation time of writing of carbon containing ink stroke to bring operability to us.We can judge according to the speed of Δ R curve decline rate and whole Δ R time curve form the formation time of writing of sample person's handwriting.
5.2, multi-times measurement method: to carry out above measurement twice with a sample.Concrete operation step is:
5.2.1, choose stroke to be checked as 5.1 kinetic measurement the record data curves that carry out a stroke resistance:
5.2.2, this sample stroke is placed 30 days naturally or artificial climate environmental cabinet in simulate the climatic environment of certain hour, again with the test condition identical with 5.2.1, again measure and record data curve;
5.2.3, more for the first time with secondary data, if data Δ R obviously diminishes for the second time, curve descending slope obviously diminishes, sample stroke writing is for writing in the recent period formation (as shown in Figure 4).
Embodiment 1: the receipt inscription time that certain part of carbon containing signature pen is write is on March 21st, 2008, through investigation, suspects that its actual formation time of writing is on May 23rd, 2012, and be on June 27th, 2012 proving time.Preliminary experiment cuts the long stroke of a segment length 2cm, and two ends are painted electrode with pencil and connected high resistant instrument.This section of stroke put into plugging meter device, and setting experimental temperature is 30 ℃.Pass into High Purity Nitrogen gas 10 minutes, valve-off cuts off High Purity Nitrogen gas, and the steam valve of fetching boiling water passes into saturated steam, opens the kinetic measurement of high resistant instrument simultaneously, and is automatically converted into Δ R value drafting time curve by software.The curve map obtaining is as shown in Figure 2:
Analyze: because Δ R value dropped to 15 from 110 within 10 second time, descending slope or the drop-out value in the unit interval are larger, so the actual formation time of writing of the person's handwriting of this receipt is nearer, are not to write for far away 2008 years.
Embodiment 2: the guarantee agreement inscription time that certain carbon containing signature pen is write is in November, 2009, through investigation, suspect that its true writing time is in May, 2012, and be on July 10th, 2012 proving time.Cut several sections of strokes and connect with pencil, wherein stroke total length is about 2cm, and two ends are painted electrode with pencil and connected high resistant instrument.This section of stroke put into plugging meter device, and setting experimental temperature is 30 ℃.Pass into High Purity Nitrogen gas 10 minutes, valve-off cuts off High Purity Nitrogen gas, and the steam valve of fetching boiling water passes into saturated steam, opens the kinetic measurement of high resistant instrument simultaneously, and is automatically converted into Δ R value drafting time curve by software.The curve map obtaining is as shown in Figure 3:
Analyze: because Δ R value dropped to 5 left and right from 25 within 10 second time, descending slope or the drop-out value in the unit interval are less, therefore the actual formation time of writing of person's handwriting of this guarantee agreement is far away, and the condition of getting rid of artificial aging should not be to write afterwards in May, 2012, but the time far away writes.
Embodiment 3: the bar that certain carbon containing signature pen is write is in January, 2011 according to the inscription time, through investigation, suspect that its actual writing time is in April, 2012, and be on June 10th, 2012 proving time.Cut several sections of strokes and connect with pencil, wherein stroke total length is about 2cm, and two ends are painted electrode with pencil and connected high resistant instrument.This section of stroke put into plugging meter device, and setting experimental temperature is 30 ℃.Pass into High Purity Nitrogen gas 10 minutes, valve-off cuts off High Purity Nitrogen gas, and the steam valve of fetching boiling water passes into saturated steam, opens the kinetic measurement of high resistant instrument simultaneously, and is automatically converted into Δ R value drafting time curve by software, obtains curve 1.Sample stroke is taken out, naturally places after 30 days, on July 10th, 2012, again this sample is carried out drawing time curve with last time testing same operation, obtain curve as shown in Figure 4:
Analyze: because the Δ R value of curve 1 changes the Δ R value variation that is obviously greater than curve 2, measure for the first time stroke resistance change very large, after placing 30 days, resistance change obviously diminishes, both relatively find that carbon containing stroke resistance in detection period is still unstable, illustrate that sample stroke writes formation time in the near future.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (7)
1. by measuring a method for stroke conductivity checks carbon containing ink writing writing time, it is characterized in that comprising the following steps:
Stroke to be checked is positioned in airtight humiture environment, after its stable conductivity, with conductivity measurement device measuring, goes out the electric conductivity numerical value of this stroke to be checked in current environment; Then change temperature or the humidity of this closed environment, the electric conductivity numerical value of this stroke to be checked is changed, record within a certain period of time the rate of change of the electric conductivity numerical value of this stroke to be checked, and draw its electric conductivity curve map corresponding with the time simultaneously; If this electric conductivity curvilinear motion amplitude is larger, judge that this stroke to be checked is to write in the recent period formation; If it is less that electric conductivity changes, judge that this stroke to be checked is to write formation long term.
2. a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time according to claim 1, it is characterized in that: described conductivity measurement equipment be high resistant instrument, conductivity meter or, micro current instrument.
3. a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time according to claim 1, it is characterized in that: the range of humidity variation of described closed environment is 0.01%～100%RH.
4. a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time according to claim 1, it is characterized in that: the range of temperature of described closed environment is 10 ℃～40 ℃.
5. a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time according to claim 1, it is characterized in that: described closed environment is closed container or humiture environmental test chamber.
6. a kind of by measuring the method for stroke conductivity checks carbon containing ink writing writing time according to claim 1, it is characterized in that comprising the following steps:
(1) choose stroke: the carbon containing ink writing stroke that selection length is 2cm～5cm is as stroke to be checked, as inadequate in stroke length, while being less than the stroke section of 2cm for several, can adopt HB or the Pencil with 2B hardness that electric conductivity is stronger that several adjacent short stroke sections are connected into the long stroke segmented mode that meets above-mentioned length, form the circuit with graphite line series connection carbon element stroke; At the two ends of stroke, with pencil contact pen, draw a picture out graphite linings that diameter is greater than 2mm as electrode;
(2) image data: described stroke to be checked is positioned in a closed container or humiture environmental test chamber, and setting its internal temperature is 30 ℃; Two potential electrode of high resistant instrument, conductivity meter or micro current instrument are closely pressed in respectively in the two end electrodes of this stroke circuit, and to continue to pass into temperature be that the High Purity Nitrogen gas of 30 ℃ is dried, in the time of the 10th minute, humidity is 0.01%RH, its stable conductivity, starts to continue to record resistance data 100 seconds; Then the water vapor that to pass into temperature and be 30 ℃, humidity be 100%RH, starts when importing water vapor to carry out the dynamic acquisition resistance data line item of going forward side by side every 2 Miao Weiyige chronomeres, in the time of the 100th second, stops;
(3) detect data: the stroke resistance value to be checked measuring, within the unit interval, significant change can occur, and gets its absolute value after passing into saturated steam; Resistance value R2 with next chronomere, the resistance value R1 of Jian Shangyige chronomere, except the above Yi Ge resistance value R1 of chronomere, be defined as resistance change rate △ R: first 2 seconds is △ R1, and second 2 seconds is △ R2 ... drawing out horizontal ordinate is that detection time, ordinate are the electric conductivity curve map of △ R;
If this electric conductivity curvilinear motion amplitude is larger, judge that this stroke to be checked is to write in the recent period formation; If it is less that electric conductivity changes, judge that stroke to be checked is to write formation long term.
7. one kind is passed through the method for double measurement stroke conductivity checks carbon containing ink writing writing time, it is characterized in that comprising the following steps: stroke to be checked is positioned in airtight humiture environment, after its stable conductivity, with conductivity measurement device measuring, go out the electric conductivity numerical value of this stroke to be checked in current environment; Then change temperature or the humidity of this closed environment, the electric conductivity numerical value of this stroke to be checked is changed, record within a certain period of time the rate of change of the electric conductivity numerical value of this stroke to be checked, and draw its electric conductivity curve map corresponding with the time simultaneously; This stroke to be checked is placed 30 days or in artificial climate environmental cabinet, simulated the climatic environment of certain hour, again with the same terms method, measure, the electric conductivity curve map that compares twice stroke to be checked, if measure for the second time its electric conductivity variation, be significantly less than the numerical value of measuring for the first time, or the curve descending slope of drawing is significantly less than primary descending slope, judge that this stroke to be checked is to write in the recent period formation.
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| CN201210274504.3A CN102818823B (en) | 2012-07-26 | 2012-07-26 | Method for detecting writing time of carbon-containing ink handwriting by measuring electrical conductivity of stroke |
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| CN103076387B (en) * | 2013-01-11 | 2015-01-14 | 同济大学 | Identification method for writing time based on DART-TOF technique |
| CN108896491A (en) * | 2018-06-22 | 2018-11-27 | 林静 | A method of identification ink forms the time |
| CN111678974B (en) * | 2020-02-04 | 2023-08-15 | 公安部物证鉴定中心 | Mass spectrum imaging analysis method for time sequence identification or auxiliary identification of cinnabar |
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| CN202083657U (en) * | 2011-05-11 | 2011-12-21 | 黄建同 | Revision and addition writing discriminating instrument for black writing |
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