WO2008148964A2 - Indicator indicating that a temperature threshold has been crossed - Google Patents

Indicator indicating that a temperature threshold has been crossed Download PDF

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Publication number
WO2008148964A2
WO2008148964A2 PCT/FR2008/050716 FR2008050716W WO2008148964A2 WO 2008148964 A2 WO2008148964 A2 WO 2008148964A2 FR 2008050716 W FR2008050716 W FR 2008050716W WO 2008148964 A2 WO2008148964 A2 WO 2008148964A2
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WO
WIPO (PCT)
Prior art keywords
state
compound
temperature
colorless
colored
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Application number
PCT/FR2008/050716
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French (fr)
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WO2008148964A3 (en
Inventor
Renaud Vaillant
Catherine Bonaiti-Fleurie
Frédéric Chaput
Original Assignee
Sa Cryolog
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Priority to US91277007P priority Critical
Priority to US60/912,770 priority
Priority to US91606107P priority
Priority to US60/916,061 priority
Priority to FR0756814A priority patent/FR2919721B1/en
Priority to FR0756814 priority
Application filed by Sa Cryolog filed Critical Sa Cryolog
Publication of WO2008148964A2 publication Critical patent/WO2008148964A2/en
Publication of WO2008148964A3 publication Critical patent/WO2008148964A3/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01KMEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K11/00Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
    • G01K11/12Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using change of colour or translucency

Abstract

The invention relates to a temperature crossing indicator making it possible to establish whether a product, particularly a perishable product, has crossed a threshold temperature value, in an increasing or decreasing direction manner, the indicator comprising: a first reversible thermochromic compound (A) having, depending on the temperature and its history of variations, either a coloured state (IU) or a colourless or slightly coloured state (U), the transition from one state to the other occurring at two distinct temperatures depending on whether the temperature varies in an increasing or decreasing manner, a second thermochromic compound (B) having, depending on the temperature and its history of variations, either a coloured state (HB) or a colourless or slightly coloured state (IB), the second compound being such that its transition to the coloured state (HB) compensates for the transition to the colourless state (U) of the first compound.

Description

 TEMPERATURE THRESHOLD TEMPERATURE THRESHOLD

The present invention relates to a control of crossing a temperature threshold, downward and / or upward, using a reversible thermochromic compound.

Such cookies, or indicators, are useful for monitoring any perishable products or substances that need to be stored under specified temperature conditions. It is primarily concerned with the agri-food sector, especially for all fresh or frozen products, but also the pharmaceutical and medical fields, some drugs to be kept at a given temperature, as well as some vaccines, blood bags ...

It is known to use a reversible thermochromic compound, having a hysteresis curve for the variation of the color as a function of temperature, to produce a temperature threshold crossing control. These controls use the properties of certain thermochromic compounds, which have a memory effect of their coloring over a greater or lesser temperature range after they have undergone a color change. FIG. 1 shows the ideal evolution of the coloration of such a compound as a function of the temperature and the thermal history of this compound. It can be seen in this figure that the compound can take two distinct states of coloration (I and II) and that, depending on the direction of change of state (increase or decrease in temperature), the change is made at temperatures T hau t e and T ba sse are also distinct or even far apart (the difference ΔT can reach sixty degrees). This difference between the high and low state change temperatures characterizes the width of the hysteresis cycle of this thermochromic compound, and it is this large width that makes it possible to use such a compound to produce a threshold crossing indicator. Indeed, if one places oneself under certain conditions, for example in a restricted temperature range comprising only one of the two change of state temperature of the compound, then any change of state of the compound in this irreversible interval. In other words, the reversibility of the color change of the compound over an unbounded temperature range is potentially irreversible over some bounded temperature ranges. If one refers again to Figure 1, for example shows that if the temperature is less than T hau t e and the system is in state I, then any intervening change in color in this interval will necessarily : i) following a temperature drop, ii) from state I to state II, iii) irreversible, since the compound will always remain below the high change temperature T hau t e , and therefore can not return in the state I. In practice, the compound will therefore be chosen so that its low state change temperature is close to or equal to / at the threshold temperature which it is desired to monitor the crossing.

These three points are valid, mutatis mutandis, if one places oneself in a temperature range comprising Thaute and not including Tbasse, which then makes it possible to use the compound as a threshold crossing control on the rise.

Such use of thermochromic compounds, however, has a significant disadvantage: the reversibility of the change of state of these compounds. Indeed, even if this one is "circumvented" by the use which is made of these compounds, this one remains very real and raises problems of confidence and thus of security of the witnesses.

Thus, FIG. 2 represents the change of state cycle of a compound having change temperatures of 0 ° C. and 30 ° C. respectively. It can be used to produce a lower threshold crossing control, for example to monitor that vaccines do not cross the temperature of 0 0 C. Indeed, some vaccines must be kept at a temperature close to 5 ° C, and their storage temperature should not fall below 0 0 C, otherwise the vaccine may be damaged. If such a scenario occurs, this would involve a change in the color of the compound (passage from state I, colorless, to state II, very colored) which would be visible and would indicate to the persons concerned that the vaccine is damaged. However, it can be seen in FIG. 2 that, if, after being lowered below 0 ° C., the storage temperature rises above 30 ° C. (ie the high change temperature of the thermochromic compound), then it is modified again the color of the witness (who returns to his state I). If the temperature then stabilizes at its nominal value of about 5 ° C, then the control shows no coloration. The information provided by the witness is therefore erroneous because it is in its initial state while the vaccine has successively reached two critical temperatures, 0 0 C and 30 0 C: although the witness displays the contrary information, the vaccine is in unusable reality.

There is therefore a serious problem of trust regarding the use of this type of witness, especially since the scenario described above can occur not only accidentally, because of dysfunctions in the conservation system, but also voluntarily and fraudulently. Indeed, it is necessary to consider that a person responsible for the storage of products which would have been mistakenly subjected to forbidden temperatures can voluntarily heat (or cool according to the type of witness) the samples in order to make disappear the coloration which would have indicated a defect of conservation, with consequent loss of stock. The object of the invention is to overcome the drawbacks described above by proposing a temperature threshold crossing control using a reversible thermochromic compound, the information of which is provided that can not be tampered with, thereby guaranteeing complete safety as regards the good preservation of the products concerned. Thus, the invention relates to a temperature crossing indicator, making it possible to establish whether a product, in particular a perishable product, has passed at least one of two threshold temperature values forming the lower and upper ends of a range of surveillance, the witness comprising: a first reversible thermochromic compound having, depending on the temperature and its history of variations, either a colored state or a colorless or slightly colored state, the transition from one state to another occurring at two different temperatures depending on the temperature varies in increasing or decreasing

a second thermochromic compound having, depending on the temperature and its history of variations, either a colored state or a colorless or slightly colored state,

the first compound being in an initial state, at a temperature comprised between the two threshold values, colored or colorless, a change of state occurring when one of the two threshold values is crossed,

the second compound being in an initial state, at a temperature between the two threshold values, colored or colorless, a change of state occurring during the crossing of the second threshold value, in the opposite direction to the crossing of the first threshold value; , before the first compound returns to its initial state, so that at least one of the two compounds is no longer in its initial state when one of the two threshold temperatures has been crossed, temporarily or not. Thus, thanks to the invention, any accidental discoloration of the first compound occurring after a coloration following the crossing of a threshold temperature is surely compensated by the prior or simultaneous coloring of the second compound. The witness according to the invention thus has a total reliability as to the information it provides on the good or bad conservation of the monitored product. Indeed, the control will be definitively colored as soon as the storage temperature of the product has crossed, even temporarily, one of the two temperatures forming the ends of the monitoring range.

In one embodiment, the color change of the second thermochromic compound is irreversible.

In one embodiment, the change of state temperature of the second compound is:

- less than or equal to the temperature of transition from the colored state to the colorless state of the first compound if this passage takes place according to an increasing temperature variation; - greater than or equal to the temperature of transition from the colored state to the colorless state of the first compound if this passage takes place according to a decreasing temperature variation.

In one embodiment, the second compound is a reversible thermochromic compound.

In one embodiment, the initial state of the first and second compounds is the colorless state.

In one embodiment, the first and second compounds are such that: the temperature of transition from the colored state to the colorless state of the second compound is less than or equal to the transition temperature from the colorless state to the colored state of the first compound.

the temperature of transition from the colorless state to the colored state of the second compound is between the two change-of-state temperatures of the first compound.

In one embodiment, the initial state of the first and second compounds is the colored state.

In one embodiment, the first and second compounds are such that: the temperature of transition from the colorless state to the colored state of the second compound is greater than the transition temperature from the colored state to the colorless state of the first compound; compound,

the temperature of transition from the colored state to the colorless state of the second compound is between the two change of state temperatures of the first compound.

In one embodiment, the transition temperatures from the colorless state to the colored state and from the colored state to the colorless state of the second compound respectively coincide with the transition temperatures from the colored state to the colorless state. and passing from the colorless state to the colored state of the first compound.

In one embodiment, the second compound comprises a thermochromic ink and / or a spin transition compound.

In one embodiment, the first compound comprises a thermochromic ink and / or a spin transition compound. In one embodiment, the first and second compounds are identical and packaged during manufacture of the control each in a different initial staining state, one being colorless while the other is stained.

In one embodiment, the first and second compounds are arranged to form a pattern.

In one embodiment, the first compound passes from the colorless state to the colored state as the temperature increases.

In one embodiment, the first compound passes from the colorless state to the colored state as the temperature varies in a decreasing manner. In one embodiment the control comprises two films of which at least one is partially transparent, the two films being hermetically assembled to contain the first and the second compounds.

In one embodiment, the first and second compounds are packaged in two separate compartments. Other features and advantages of the invention will appear with the description given below, the latter being carried out for descriptive and non-limiting purposes with reference to the following figures in which:

FIGS. 1 and 2, already described, represent the coloring cycle as a function of the temperature of a reversible thermochromic compound;

FIG. 3 represents the spin state change cycle as a function of the temperature of a spin transition compound;

FIG. 4 represents an example of use of a control according to the invention; FIG. 5 represents the color variation of a control according to the invention when the change of state of the second thermochromic compound is irreversible;

FIGS. 6, 7 and 8 represent different combinations of the first and second compounds when the change of state of the second compound is reversible;

FIG. 9 represents an embodiment of the invention in which two identical compounds are used in different starting states.

With reference to FIGS. 4 to 9, several embodiments of a threshold crossing control device according to the invention, capable of detecting a "downward" crossing and / or "Rise", that is to say to detect the crossing of a low temperature limit and / or a high limit. Thus, as shown in FIG. 4, the control 10 is in the form of a colorless label, in the self-adhesive example, intended to be affixed to each product to be monitored. According to the invention, the control 10 comprises a first reversible thermochromic compound A and a second thermochromic compound B. To produce the compound A, a thermochromic ink can be used, for example as those described in the documents EP1657073 and US5,558,699.

According to the invention, the coloring of compound B must take place at a predetermined temperature, so as to be able to compensate for a possible change to the colorless state of compound A if the successive temperature variations have had the consequence that after crossing the temperature threshold, compound A described a complete cycle of staining / discoloration. The examples described below show that in addition to providing absolute security to the control, the presence of a second thermochromic compound B makes it possible to produce a control which provides both downward and upward monitoring, allowing ensure that the temperature has remained within a given range or monitoring range.

In the example of Figure 4, the compounds A and B are trapped in two separate compartments of the control 10, which thus has two viewing windows juxtaposed. As can be seen in FIG. 4, the reading of the control is very simple: since the initial state of the two compounds A and B is the colorless state, there has been a lack of conservation since at least the one of the windows displays a color. Alternatively, the compounds A and B can be combined in a single package, as long as their mixing is possible without affecting the operation of the control.

The control described in this example is carried out so as to monitor the vaccines described above with reference to FIG. 2. Thus, FIGS. 5 and 6 show that compound A is identical to the compound used in the example of FIG. FIG. 2: it moves from the colorless or slightly colored state (state I A ) to the colored state (state II A ) at a temperature T ba sse-A close to zero degrees Celsius, thus making it possible to "mark" the vaccine if it has been stored at a temperature below 0 ° C, even temporarily. According to the invention, the control 10 also comprises a second thermochromic compound B, reversible or not. FIG. 5 describes an embodiment of the invention where the second thermochromic compound B has an irreversible state change. Compound B is chosen so that its temperature T hau t e -B of transition from the colorless state (state I B ) to the colored state (state II B ) is less than or equal to the temperature of inverse passage T hau t e -A compound A. Thus, if the monitored product (state 1) crossed the threshold 0 O C (condition A 2, A staining), and the temperature then exceeds thirty degrees, then the compound A will again become colorless (state 4 A ), but, shortly before or at the same time, compound B will stain irreversibly (state 3 A ). Thus, the coloring of the control window 10 corresponding to the compartment containing the compound B will be final, regardless of the subsequent variations in the storage temperature. The witness will therefore clearly and clearly indicate to the persons concerned that the monitored product is damaged and should not be used. In the example, the monitoring range of the indicator 10 is defined by the temperatures T ba sse-A and T hau te-B-

Figures 6, 7 and 8 show different variants of an embodiment of the invention wherein compound B is a reversible thermochromic compound. In this case, it has two change temperatures T low eB and T high -B, and the different variants presented below depend on the relative values of these temperatures with respect to the change of state temperatures of the first compound A.

FIG. 6 shows a variant in which the low TB and T high -B T-state change temperatures of the second B compound are such that each change of state of the compound B coincides with the inverse change of the compound A. In other words, T basS eB is equal to T low- A (or very close to T low- A) and T hau t e- B is equal to T hau t e- A (or very close to T hau t e - A) - Thus, the control 10 works in the same way as in Figure 5, except that when the temperature exceeds T high- B and compound B becomes colored (the compound A becoming colorless), the coloring of compound B is not definitive. Indeed, if the temperature is brought down below T low eB, then the compound B becomes colorless again. However, the security provided by the control according to the invention is always complete because, at the same time, compound A becomes colored again. The indicator will be colored if one of status change Lower temperatures T A or T B Upper, the compound A, has been crossed. In this example, these are the two change temperatures state of the first compound A which define the monitoring range of the control 10. As will be seen in the following examples, it is not necessary that the change of state temperature of the compound B coincide with the change temperatures. reverse state of compound A for the control to operate.

In fact, FIG. 7 represents a variant in which the second compound B is such that its change of state temperatures T ba sse-B and T high - B are respectively lower than the inverse change temperature of the compound A. In other words, T ba sse-B is less than or equal to Tbasse-A and T hau te-B is less than or equal T hau t e -A- The advantage of this configuration is in particular to obtain, with a even compound a, a different tracking range to that of the example of Figure 6. in the present example, the monitoring range, narrower, is defined by the Bass T eA and Th temperatures ute-B- witness however, works in the same way: the initial state of the two compounds A and B is the colorless state (state 1). If the control passes the temperature Th at te-B, which sets the high limit of the monitoring range of the control, then compound B changes to the colored state (state 2B ). If this overshoot is important (state 3 B ), compound B remains colored while compound A does not change state and remains in a colorless state. If then the temperature decreases and it crosses the lower limit of the monitoring range T basS eA, then the compound A will go to the colored state. Both compounds A and B will then both be in a colored state (state 4B ). If the temperature continues to fall and becomes lower than T low eB, then compound B will go back to a colorless state while compound A remains colored (state B ). If, subsequently, the temperature rises and stabilizes within the monitoring range, compound A will still be colored. The security of the witness is therefore absolute: as soon as at least one of the temperature limits of the monitoring range will be crossed, even temporarily and for a short period of time, then at least one of the compounds A or B will be colored. The variant of FIG. 7 further shows that the control can be adapted in a simple manner by combining thermochromic compounds and their change of state temperatures in order to precisely define the desired monitoring page.

A third variant is shown in Figure 8. Unlike the variants shown in Figures 6 and 7, the initial state of the compounds A and B is in this example the colored state. In this example, the The temperature of the change of state T ba sse-B and T hau t e -B of the second compound B are respectively greater than each inverse change temperature of the compound A. In other words, T ba sse-B is greater than or equal to Tbasse-A and T hau te-B is greater than or equal to T ue t e -A- It is therefore the temperatures T low eB and T high -A which define here the monitoring range. Since the initial state of the two compounds is the colored state, the control will indicate that there has been a defect of conservation if at least one of the two compounds is in the colorless state, and not in the colored state as for the variants of Figures 6 and 7. For the rest, the operation is identical to the variants of the aforementioned figures.

As shown by the examples described above, the control according to the invention makes it possible to monitor the exceeding of a temperature threshold upwards or downwards with total security as to the information provided by the witness: no falsification or accidentally erroneous information is possible as for the indicators of the prior art.

Alternatively, at least one of the thermochromic compounds used comprises a spin-transition compound, for example those described in document FR2755696. Figure 3 shows an example of a hysteresis loop of spin transition compounds. On the ordinate, a magnitude has been reported which reflects the spin state and not the color state; the state of coloration exhibits an inverted hysteresis cycle comparable to that represented in FIG. 1. These compounds exhibit a transition of spin states, between a so-called low spin state (LS) and a so-called high spin state (HS) which is induced thermally, and that is accompanied by electronic configuration change and structural modifications of the molecules causing an abrupt change in the absorption spectrum of the molecules, and therefore the color of the compounds. Thus, in the example, the compounds are purple in the low spin state (LS), whereas in the high spin state (HS) these compounds are white.

In another variant, to produce the control 10, two identical reversible thermochromic compounds A and A ', of the type represented in FIG. 1, are used, but brought during the manufacturing each in a different initial state from each other. . Thus, the compound A will be in the initial state I, while the compound A 'will be in the initial state II.

In a first example, the compounds A and A 'are packaged in two separate compartments, as for the example of FIG. Thus, before use, the window of the compartment containing A does not display coloring, while the second window, that of the compartment containing A ', displays a coloration. The two windows thus indicate states of opposite colorations. The control 10 is then affixed to a product to be monitored. The operation of the control 10 is then as follows: i) if the temperature thereof exceeds T hau t e -A, then the compound A 'will go from the state II to the I state, while the compound A does not change its state (state I). The two windows will then indicate the same coloring state, in this case the colorless state. ii) if, on the contrary, the temperature of the monitored product falls below T ba sse-A, then the compound A goes from state I to state

II while the compound A 'does not modify its state (state II). The two windows will then indicate an identical state: the colored state. (iii) if the case referred to in subparagraph (ii) occurs after the change in temperature has already occurred for the first time in the case referred to in subparagraph (i), the result will be identical because then the two compounds pass jointly from the state I to state II when crossing T basS e- iv) Idem, mutatis mutandis, if cases ii) and i) occur successively in this order.

It is therefore seen that, if it is different from the other examples, the reading of the control remains always simple: there will be here lack of conservation since the coloration of the two windows is identical, whatever the state of coloration. The monitoring range is here defined by the interval between T ba sse-A and T high eA-

In a second example, represented in FIG. 9, the compounds A and A 'are trapped in the same package, and these are packaged during manufacture in such a way that their difference in color forms a pattern, in the example in the shape of a cross. For example, the control of FIG. 9 can be obtained by using compound A, deposited in its II state (colored) at ambient temperature, and by heating the part intended to form the pattern locally, which then becomes transparent. In the example shown in FIG. 9, the change of state temperatures of compound A

(or A ') are + 1 ° C and + 15 ° C. Before use, the indicator 10 therefore has a single viewing window displaying a pattern. So we see that if the temperature exceeds the temperature T hau t e -A, the portion of the control in the colored state will pass to the colorless state, the surface of the control 10 will be completely colorless. Conversely, if the temperature exceeds the temperature T ba sse-A, then the portion of the control in the colorless state will change to the colored state, the witness then being fully colored. The witness of FIG. 9 will therefore indicate a defect of conservation since it no longer makes it possible to discern any motive, whether the state indicated is colorless or colored.

Claims

1. Temperature crossing indicator (10), used to establish whether a product, particularly a perishable product, has passed at least one of two threshold temperature values forming the lower and upper ends of a monitoring range, the control (10) comprising:
a first reversible thermochromic compound (A) exhibiting, depending on the temperature and its history of variations, either a colored state (IU) or a colorless (U) state or little color, the transition from one state to another intervening at two different temperatures depending on whether the temperature is increasing or decreasing,
a second thermochromic compound (B) exhibiting, depending on the temperature and its history of variations, either a colored state (HB) or a colorless (IB) state or a slightly colored state,
the first compound (A) being in an initial state, at a temperature lying between the two threshold values, colored (IU) or colorless (U), a change of state occurring when crossing one of the two threshold values,
the second compound (B) being in an initial state, at a temperature between the two threshold values, colored (HB) OR colorless (IB), a change of state occurring during the crossing of the second threshold value, in the opposite direction of the crossing of the first threshold value, before the first compound (A) returns to its initial state, so that at least one of the two compounds is no longer in its initial state when a both threshold temperatures have been crossed, temporarily or not.
The control (10) of claim 1, wherein the color change of the second thermochromic compound (B) is irreversible.
The control (10) of claim 2, wherein the change of state temperature of the second compound (B) is:
- less than or equal to the temperature of transition from the colored state (IU) to the colorless state (U) of the first compound (A) if this passage takes place according to an increasing temperature variation; - greater than or equal to the temperature of transition from the colored state (IU) to the colorless state (U) of the first compound (A) if this transition takes place according to a decreasing temperature variation
4. The control of claim 1, wherein the second compound (B) is a reversible thermochromic compound.
5. The control of claim 4, wherein the initial state of the first and second compounds (A, B) is the colorless state.
The indicator (10) of claim 5, wherein:
the temperature of transition from the colored state (HB) to the colorless state (IB) of the second compound (B) is less than or equal to the transition temperature from the colorless state (U) to the colored state ( IU) of the first compound (A).
- The temperature of transition from the colorless state (IB) to the colored state (IIB) of the second compound (B) is between the two change of state temperature of the first compound (A).
The indicator according to claim 1, wherein the initial state of the first and second compounds (A, B) is the colored state.
8. The control of claim 7, wherein:
- The transition temperature from the colorless state (IB) to the colored state (IIB) of the second compound (B) is greater than the transition temperature from the colored state (IU) to the colorless state (U) of the first compound (A),
the temperature of transition from the colored state (IIB) to the colorless state (IB) of the second compound (B) is between the two change of state temperatures of the first compound (A).
9. Control according to claim 5 or 7, wherein the transition temperatures from the colorless state (IB) to the colored state (IIB) and transition from the colored state (HB) to the colorless state (IB). of the second compound (B) coincide respectively with the transition temperatures from the colored state (IU) to the colorless state (U) and from the colorless state (U) to the colored state (IU) of the first compound (A).
10. The indicator (10) according to one of claims 4 to 9, wherein the second compound (B) comprises a thermochromic ink and / or a spin transition compound.
11. The light (10) according to one of claims 1 to 10, wherein the first compound (A) comprises a thermochromic ink and / or a spin transition compound.
The control (10) according to claim 10 or 11, wherein the first and second compounds (A, B) are identical and packaged in the manufacture of the control (10) each in a different initial staining state, one being colorless while the other is colored.
13. A control according to claim 12, wherein the first and second compounds (A, B) are arranged to form a pattern.
14. Indicator (10) according to one of the preceding claims, wherein the first compound (A) goes from the colorless state (U) to the colored state (IU) when the temperature varies increasingly.
15. Indicator (10) according to one of claims 1 to 13, wherein the first compound (A) goes from the colorless state (U) to the colored state (IU) when the temperature varies decreasingly.
16. Indicator (10) according to one of the preceding claims, comprising two films, at least one of which is partially transparent, the two films being assembled hermetically to contain the first and the second compounds (A, B).
17. Control (10) according to one of the preceding claims, wherein the first and the second compounds (A, B) are packaged in two separate compartments.
PCT/FR2008/050716 2007-04-19 2008-04-21 Indicator indicating that a temperature threshold has been crossed WO2008148964A2 (en)

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US91277007P true 2007-04-19 2007-04-19
US60/912,770 2007-04-19
US91606107P true 2007-05-04 2007-05-04
US60/916,061 2007-05-04
FR0756814 2007-07-30
FR0756814A FR2919721B1 (en) 2007-07-30 2007-07-30 Crossing indicator with temperature threshold

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