阅读说明：本技术 用于准备液体的蒸馏测量的设备和方法及液体分析系统 (For preparing the device and method and liquid analysis system of the distillation measurement of liquid ) 是由 弗兰克·齐默尔曼 卡斯滕·金特 丹尼尔·佩尔甘德 于 2019-05-15 设计创作，主要内容包括：本发明提供用于准备液体的蒸馏测量的设备(100)和方法及液体分析系统,所述设备具有：加热器(101),从一组标准化的孔板(203a、203b、203c、203d)中选择的一个孔板(103、203a)能放置到所述加热器上,并且所述加热器构成为用于加热包含液体(107)的、放置到孔板(103)上的容器(105),以用于实施标准化试验以确定液体的蒸发特性；特别是电气的移动系统(110),所述移动系统构成为用于使加热器(101)移动并且当放置到加热器(101)上的孔板(103)向容器(105)的压紧力(F)达到阈值时中断加热器(101)的进一步移动。通过该设备避免操作错误并且还能够将孔板精确地且无错误地定位在烧瓶上,阻止玻璃烧瓶由于从下方通过孔板传递的过高的力作用而损坏。(The present invention is provided to prepare the equipment (100) of the distillation measurement of liquid and method and liquid analysis system, the equipment includes heater (101), the orifice plate (103,203a) selected from one group of standardized orifice plate (203a, 203b, 203c, 203d) can be placed on the heater, and the heater is structured to container (105) that heating includes liquid (107), being placed on orifice plate (103), to test the evaporation characteristic to determine liquid for execution standardization；Especially electrical mobile system (110), the mobile system are structured to the further movement for keeping heater (101) mobile and interrupting heater (101) when the orifice plate (103) being placed on heater (101) reaches threshold value to the pressing force (F) of container (105).Operating mistake is avoided by the equipment and orifice plate can also accurately and be without error located on flask, prevents glass flask due to acting on damage by the excessively high power that orifice plate transmits from below.)

1. a kind of for preparing the equipment (100) of the distillation measurement of liquid, comprising:

Heater (101), the orifice plate that can be selected from one group of standardized orifice plate (203a, 203b, 203c, 203d) (103,203a) are placed on the heater, and the heater is structured to heating and includes liquid (107), placement Container (105) on to orifice plate (103), to test the evaporation characteristic to determine liquid for execution standardization；

Mobile system (110), especially electrical mobile system (110), the mobile system are structured to make heater (101) mobile, and if the orifice plate (103) being placed on heater (101) reaches threshold to the pressing force (F) of container (105) Value interrupts the further movement of heater (101).

2. equipment described in accordance with the claim 1, wherein the mobile system (110) includes moveable support system (133), heater (101) is kept by the support system, wherein the equipment is structured to monitor and/or determine instruction Along the length of movement routine and/or the parameter of position (z) of support system (133), particularly the stepping of stepper motor (151) Amount.

3. equipment according to claim 1 or 2, wherein the equipment is structured to make support system (133) from bracket The initial position (za) of system, particularly the starting position of pre-determining set out and are moved to final position (ze), in the most final position The place's of setting pressing force (F) reaches threshold value,

Wherein, the parameter of position that be allocated to initial position (za), that instruction moves along path has the first value (w1), and

The parameter of position that be allocated to final position (ze), that instruction moves along path has second value (w2),

Wherein, the equipment is configured to, for calculating the difference of the first value and second value, as the movement routine for indicating to pass through at this time The difference of length.

4. equipment described in accordance with the claim 3, wherein the equipment is also configured as:

Based on the difference, (Δ z), particularly also type and/or parameter and/or identifier based on container (105), are inferred to The type and/or parameter and/or identifier of orifice plate (103) and/or its auditorial and/or vision prompt system is mentioned Show；And/or

Based on the difference (Δ z) be inferred to orifice plate (103) type and/or parameter and/or identifier and/or by it by listening Prompt system feel and/or vision prompts；And/or it is inferred to the type and/or parameter and/or identifier of container (105) And/or its auditorial and/or vision prompt system is prompted.

5. equipment according to claim 1 or 2, wherein the equipment is also configured as:

User can be allowed to select the desired test to be implemented from the selection to standardized assays；And/or

Allow user that selected orifice plate is placed on heater；And/or

In heating system it is mobile until interrupting after, if it is determined that orifice plate and/or the movement routine length passed through not with institute The test of selection is mutually compatible with, then indicating alarm.

6. equipment according to claim 1 or 2, wherein the mobile system includes

Stepper motor (151)；

Lead screw (153) driven by stepper motors, especially along the lead screw of track (143) setting.

7. equipment according to claim 2, wherein the support system (133) includes

Supporting member (139), heater (101) are supported by the supporting member；

Moving element (141), the moving element act on lead screw (153) in order to drive and especially by track (143) Guidance；

Force measuring device (145), supporting member (139) are coupled by the force measuring device and moving element (141).

8. equipment according to claim 7, wherein the force measuring device includes

Spring (147), an end of the spring is mounted on moving element (141) and its another end is mounted on branch It holds on element (139)；

Grating (149), the grating are coupled with stepper motor (151),

Wherein, the spring (147) is compressed by the distance of definition in the threshold value of power, and thus triggering grating (149) will move System (110) is placed in stopping.

9. equipment according to claim 1 or 2, wherein the orifice plate (103) and/or the container (105) and such as subscript At least one of standardization test is mutually compatible with:

ASTM D86, ASTM D850, ASTM D1078 and ISO 1078 are at least pressed respectively in the applying date effective version,

Especially with for distillate fuel it is following specification at least one of it is mutually compatible: ASTM D86,3405 ISO, IP 123, BS200-123, JIS K 2254 and GOST 2177, respectively at least by the applying date effective version；And/or

Especially with for solvent distillation it is following specification at least one of it is mutually compatible: ASTM D1078, IP195, BS2000- 195, ASTM D850, ISO918, BS4591, JISK0066 and ISO4626, respectively at least by the applying date effective version； And/or

It is especially mutually compatible at least one of following specification: ASTM D524, IP14, BS2000-14, ISO4262, ASTM D4530 and ISO10370, respectively at least by the applying date effective version.

10. a kind of liquid analysis system (150,250), particularly automatic distillation unit, for being tried according at least one standardization The evaporation characteristic of determining liquid is tested, the liquid analysis system includes

Container (105,205) with opening, particularly with the branch for leading to condenser (269)；And

Device (120,220) for closed container, comprising:

At least one temperature measurement system, especially for measuring the vapor (steam) temperature of the liquid within container, the temperature is surveyed Amount system has bar (123,223) and temperature meter (121,221)；

A part guidance of closure member (125) with through-hole, being used for closed container (105), the bar passes through the through-hole, So that temperature meter is arranged within container (105)；

Optionally the longitudinal direction on closure member transverse to bar stretches out in the supporting element (129,229) of closure member, the branch Support member and the counterpart (131,231) of auxiliary device can push together；

According to the equipment (100,200) of the distillation measurement described in one of the claims for preparing liquid；And especially It is

Multiple standardized orifice plates (203a, 203b, 203c, 203d), the orifice plate can be placed on heater (101,201).

11. a kind of for preparing the method for the distillation measurement of liquid, comprising:

An orifice plate (203a) is selected from one group of standardized hole (203a, 203b, 203c, 203d)；

Orifice plate (203a) is placed on heater (201), the heater be structured to heating comprising liquid (207), The container (205) being placed on orifice plate (203a), to test the evaporation characteristic to determine liquid for execution standardization；

Heater (201) is mobile towards container (205)；

If the orifice plate (203a) being placed on heater (201) reaches threshold value to the pressing force (F) of container (205), interrupt It is mobile.

Technical field

The equipment that the present invention relates to a kind of for preparing the distillation measurement of liquid further relates to a kind of liquid analysis system, spy Be not automatic distillation unit, with for determining the evaporation characteristic of liquid according at least one standardized assays, and the present invention this It further relates to outside a kind of for preparing the method for the distillation measurement of liquid.

Background technique

According to the evaporation characteristic for analyzing liquid standardized assays specification regulation, according to flask size and according to The fluid sample to be studied must select four different one of orifice plates or thermal insulation board, these orifice plates or thermal insulation board must be placed into On heating device, so as to heat the flask with the sample to be studied according to normalization condition.In addition, orifice plate or heat-insulated Diametrically of the plate in the hole of plate centre is different, and circle flask is placed during standardizing measurement or during standardized assays On the edge in the hole.Here, orifice plate is placed on the heating, the heating device shifts to flask from below, until hole Plate closely closes flask from bottom side.

1 967 269 B1 of EP discloses a kind of automatic positioning equipment, and the automatic positioning equipment has relative to distilling flask Have a heating room, the positioning device with the fixed bracket in position, the heating room with heating element, a set of there is plug and structure It build the distilling flask, a set of thermal insulation board and the controller for controlling heater of thermocouple therein in.Sled via spring with Constant power is connect with heating room, is moved between the rest position and the operative position to make to heat room.It is equipped with thus for making The manually handle device that sled moves and the locking device for fixing operating position.

1 967 848 B1 of EP discloses a kind of for standardizing the code translator of the thermal insulation board of distillation apparatus, wherein each decoding Hole is introduced into thermal insulation board and based on model is distributed on the surface of decoder, and the model is dedicated for the surface. A set of sensor is arranged to corresponding decoding hole and the sensor issues detectable signal, and the detectable signal represents heat-insulated Plate, to verify, whether the isolation board for meeting the testing standard of pre-determining is placed between heating element and distilling flask in centre.

Routinely, orifice plate is selected by user before coming into effect standardized assays.It may be selected herein by user It selects the orifice plate of mistake and is placed on heating device and mistake occur.It is described using the orifice plate of mistake Test can not implement without error, particularly can not comply with standard ground or implement with meeting specification.It is described test then must in Break, correct orifice plate must be selected and be placed on heating device and must start over test.Thus the time is consumed Take and cost increase.

Summary of the invention

Therefore, the equipment and one kind that the distillation that the object of the present invention is to provide a kind of for preparing liquid measures are corresponding Method, the standardized assays for determining the evaporation characteristic of liquid can be implemented faster and more reliably with this.In particular, this The task of invention is, provides such device and method, wherein avoid operating mistake and can also by orifice plate accurately and It is located on flask without error.In particular, task of the invention lies in prevent glass flask due to excessively high power from below It acts on and damages, the power effect passes through orifice plate and transmits.

A kind of form of implementation according to the invention provides a kind of equipment that the distillation for preparing liquid measures, described to set Standby to include heater, the orifice plate selected from one group of standardized orifice plate can be placed on the heater, and be heated Device is structured to container that heating includes liquid, being placed on orifice plate, to test for execution standardization to determine liquid Evaporation characteristic；Mobile system, especially electrical mobile system, the mobile system be structured to make heater (such as It is straight up) mobile, and heating system is interrupted when the orifice plate being placed on heater reaches threshold value to the pressing force of container Further movement.

The present invention is in field distillation unit (ADU) of automatic (or normal pressure), can be according to using the distillation unit Different specification (such as ASTM D86) determines the distillation characteristic of liquid, particularly oil product or solvent.Here, the sample of specification Container, so-called flask be heated from below and the distillate that generates at this time via liquefier condenser is exported to and is caught in other words Collect in container.In addition, the distillation characteristic of liquid is characterized by means of temperature measurement.

Distillation measurement may include the standardized assays according to specification, such as ASTM specification or ISO specification.

According to the criterion of the exact definition in applicable code test, each form of implementation according to the invention will be pre- The sample for determining volume is filled into sample container (such as flask) and closes sample container to be used for closed device.Sample Product then heat under conditions of definition, so that the part of sample is evaporated.The cooling steam and within the barrel in condenser line Collect condensate.By means of the temperature and time of temperature measurement system record steam during implementing test.As standardized The result of automatic distillation test for example may include following parameter:

Initial boiling point that is, the first drop distillate drops into temperature when accommodating in cylinder

Final boiling point that is, the maximum temperature during distillation

The distillate total volume trapped in receiving cylinder

The sample remained in distillation container is remaining

It does that is, last drips temperature when distillate is evaporated from container bottom

Distillation curve.

By drawing temperature relative in the opposite recovery volume accommodated in cylinder, distillation curve can be obtained.From steaming Evaporating in curve can for example export using the boiling range of sample as the difference between maximum temperature and minimum temperature.

In particular, each form of implementation of the invention is suitable for implementing code test for distilling oil product, such as ASTM D86 (0 to 4 group), ISO3405, IP123, BS2000-123 are pressed respectively in the applying date effective version.

Each form of implementation of the invention apply also for implementing for the code test of solvent distillation, such as ASTM D1078, IP95,BS2000-195,ASTM D850.It may include the corresponding distillation of studied sample as the result for implementing test It curve and, for example, does.Test above-mentioned at least can carry out the corresponding of code test in the applying date effective version Implement.

Each form of implementation of the invention can for example support the sample to boiling range between such as 20 DEG C to 400 DEG C Standardization Research.It can especially support standard ASTM D86, ASTM D850, ASTM D1078 and ISO 3405, IP 123,195 IP, it is all respectively by the applying date effective version.Technical specification for these code tests can be in ASTM (such as www.ASTM.org) is obtained.Each form of implementation according to the invention can support 0 DEG C to 450 DEG C of vapor (steam) temperature model It encloses, 0 DEG C to 80 DEG C of condenser temperatures and 0 ° to 50 ° of chamber temperature range.In addition, may include in each form of implementation Barometric pressure sensor, the barometric pressure sensor are able to achieve, and can automatically calibrate result in normal pressure.

In particular, each form of implementation of the invention is designed as characterization oil product, especially it is different from for the de- of seawater Salt facility, the facility for being used to prepare drinking water, for the clean facilities of waste water, the chemical facilities for handling hydrocarbon, Rotary evaporator, the distillation facility for processing of biological materials.In particular, each form of implementation offer of the invention is standardized Distillation apparatus, particularly automatic distillation instrument at atmosheric pressure for fluid sample, the fluid sample especially mineral oil The sample of product, wherein the measurement of distillation parameter is implemented according to predefined testing standard, and the testing standard is from multiple possibility Standard in select, some of the above example gives these standards.

In a kind of alternative form of implementation, standardized distillation apparatus can be provided under a reduced pressure or true Sky is lower to measure distillation parameter.

Orifice plate can be made of heat-insulated material and have the hole in center or the circular void in center.Circle in the orifice plate The diameter in shape gap can be less than the diameter of container, particularly circle flask.Orifice plate can be and can reversibly connect with heater, Such as it is connected by one or more clips, thread mechanism, magnetic element or the like.Container, particularly glass circle flask (especially after orifice plate is placed on heater) can be arranged so that on orifice plate, so that the EDGE CONTACT of circular void The outer surface of spherical surface, particularly band, to realize: (part is located at the flat of orifice plate for the part of the pre-determining of circle flask Under face) be located relative to heater heating element pre-determining position in.It is thereby achieved that according to one or more The specification or standard of definition heats the liquid within container.Heater may include electrical heating elements.

The liquid be especially the mixture that can be related to a kind of mineral oil product or multi mineral oil product such as Crude oil.Other examples of liquid are, for example, solvent, the solvent in coatings industry for dilute/disperse pigment.

It may include electric component, such as motor, particularly stepper motor that the mobile system, which is especially, and the motor is used as Driving device for traveling heater.After manipulation switch, the electrical mobile system is automatically by heater to moving up It is dynamic, until the edge of the restriction circular open of orifice plate circularly contacts circle flask from below and until pressing force reaches threshold value. User's intervention manually after starting (electrically) drive system is not needed.Therefore, the equipment is configured to, by hole After plate puts heater, in this way towards the mobile heating system of flask, so that then in the further manual of not user It can be used to determine that the standard of the evaporation characteristic of liquid to be tried to prepare and then implement according at least one in the case where intervention It tests.

The mobile system is especially the means intervention next (upward) for not needing user even if traveling heater, also heating Device moves upwards.It can be to avoid faulty operation with this.(especially electrical) mobile system also can be constructed for making to heat Device is moved at the appropriate speed, for example with constant speed, and the speed avoids damage component.Mobile system also may be constructed For, for example, it is relatively large at a distance from orifice plate is between flask when relatively high movement speed is set first, the movement speed with At a distance from orifice plate is between flask reduce and gradually or step by step reduce.With this, quick preparation not only can achieve, And the risk that do not damage.

If component used in certain, particularly orifice plate and/or container are not tried with (especially selecting in advance) standard It tests and is mutually compatible with, then the equipment can acoustically and/or visually prompt the incompatibility.In addition, standardized assays Implementation can support the component of the test to prevent in normal operation by correspondingly manipulating other in this case, example Such as heater itself, temperature measurement system, analysis system, prompt system.

It can achieve with this and rapidly prepare standardized assays and can be mentioned using vicious component It warns report, so as to prevent operating mistake, particularly implement further test procedure in a wrong manner.

A kind of form of implementation according to the invention, the mobile system include moveable support system, and heater is by institute State support system holding.The equipment can be constructed for monitoring and/or determining instruction moving along support system herein The stepping-in amount of the length in path and/or the parameter of position, particularly stepper motor.

The support system be moveable, particularly can electrically move, particularly can move straight up and It is especially driven by motor for moving.The support system for example may include arm, bar, platform or these combination, so as to Such as bearing, support keep heater in other words.Support system may include multiple components, for example, with driving motor (such as through By lead screw) effect component and keep in other words support heater the second component.First assembly and the second component without going through It is rigidly connected and is mechanically connected, but can for example be connected by elastic connection, such as spring, particularly helical spring, institute Stating spring can be considered for measuring force.Pressing force can for example be measured based on the deformation of spring, such as helical spring or Such as it is measured by piezoelectric element.The threshold value can adjust according to special application or standardized assays, such as root Multiple and different standardized orifice plate and more is adjusted or can be applied to according to applied container and/or applied orifice plate A different standardized container.In particular, the threshold value can be equivalent to or equal to the testing standard according to pre-determining Scheduled pressing force.

During support system is mobile, position changes along the movement routine of support system.Movement routine for example can be Straight line that is, straight movement routine is, for example, accurate movement routine straight up.The movement routine can pass through one Or multiple tracks define and/or lead screw by being driven by motor drives.Pressing force can be along the vertical direction orifice plate with Power between flask or container.

Before mobile towards container (lower end) together with heater and orifice plate in support system, the container can be Upper end keeps (in fixed position) by one or more holding elements, without keep following container area, Especially glass circle flask.Therefore part below container can be without other holding elements.In particular, under container The space of side is freely, so that heater can non-dangerously shift to container from below together with orifice plate.In the upper surface of container Region at holding can be strong in this way, make it possible to resist according to threshold value pressing force.

Instruction can for example be provided or by step along the parameter of the position of the movement routine of support system by length unit Amount into the rotation of motor is provided or is indicated by voltage or similar value.The position for example can relative to reference position, Such as initial position defines, such as by length specification by length unit, such as millimeter or by by stepper motor or The amount of stepping or rotation that other motors complete provides.Indicate the parameter of the length of the movement routine along support system for example It can be determined by the difference of the reference position of support system and instantaneous position.The position of support system can for example be related to bracket The position of the details of the component or determination of the determination of system.In particular, the position of support system or can be related to primarily logical Cross the position of the mobile first assembly of motor, particularly motor otherwise can be related to for example via elastic element flexibly with bracket The position of second component of the first assembly connection of system.

A kind of form of implementation according to the invention, the equipment are structured to make support system from the initial of support system Position, particularly the starting position of pre-determining are moved to final position, and at the final position, pressing force reaches threshold value, In, the parameter of position that be allocated to initial position, that instruction moves along path has the first value, and is allocated to final position , the parameter of the position that instruction moves along path there is second value, wherein the equipment is structured to the first value and the The difference of two-value is calculated as the difference for the movement routine length that instruction is passed through at this time.

The final position of support system can correspond to following state, and in the state, orifice plate drives towards container completely, from And the marginal portion in the hole of orifice plate around container and especially circularly contact outer wall.Pass through the edge and container in hole The pressing force according to threshold value is transmitted in the contact of outer surface in final position.Initial position, which can be, to be passed through before entire Any position during movement routine especially can be predefined starting position.Initial position is lower than final position.For reality Apply corresponding preparation method, (electrically) mobile system is at least configured to move up heater (together with orifice plate).

In order to orifice plate and/or container can be replaced, such as after successful implementation standardized assays, the mobile system It can be constructed for that heater (together with orifice plate) is made to move down, particularly move back to again initial position, particularly open In beginning position.The speed of backhaul can be relatively low first, and to loosen orifice plate slowly with container, this is avoided the appearance The damage of device.Then, the speed of backhaul can be improved, without damaging other assemblies.In other forms of implementation, the speed It is substantially constant during backhaul.However, the speed for example can be faster than the speed during moving up.

The difference is thereby indicate that movement routine length between initial position and final position.In particular, the difference Value can be different using different orifice plates, and/or can also be using different containers It is different and especially can be respectively using the container combination different from orifice plate in pairs it is different.Cause This, can be determined clearly the combination of applied orifice plate and container based on determining difference.Therefore, the equipment can be with structure Compatibility as the code test for determining the combination of applied orifice plate and container and selecting in advance, which exists, does not still deposit And there is no for example sound an alarm in the case where compatibility.It therefore can be to avoid the mark for implementing determination with the component of mistake Standardization test.

A kind of form of implementation according to the invention, the equipment are also configured as based on difference, particularly also based on appearance The type and/or parameter and/or identifier of device are inferred to the type of orifice plate and/or parameter and/or identifier and/or are passed through The sense of hearing and/or vision prompt system prompts；And/or the type and/or parameter and/or mark of orifice plate are inferred to based on difference Know and accords with and/or prompt its auditorial and/or vision prompt system；And/or it is inferred to the type and/or ginseng of container Amount and/or identifier and/or its auditorial and/or vision prompt system is prompted.

The type of the container can for example be defined by type mark, such as manufacturer and model.Parameter for example may be used It is defined with the diameter by spherical circle flask or the volume by container or capacity.The identifier of container may include container Specific mark.Similarly, these parameters can be defined for orifice plate.The parameter of orifice plate for example can by following parameter, Such as the diameter of the circular void within orifice plate defines.The equipment therefore can be at least such that ground be constituted, so that from true Fixed movement routine especially from the parameter of at least one instruction movement routine and is based particularly on difference and determines, hole Whether plate has been placed on the heaters, and orifice plate is mutually compatible with one of multiple standardsization test and can select the standardization in advance Test.

A kind of form of implementation according to the invention, the equipment are also configured as: user can be allowed to standardized assays The desired test to be implemented is selected in selection；And/or allow user that selected orifice plate is placed on heater； And/or by heating system it is mobile until interrupting after, if it is determined that orifice plate and/or process movement routine length not with institute The test of selection is mutually compatible with, then indicating alarm.It is hereby ensured that selected desired standardized test is really with configuration Implement to the component of the test.

A kind of form of implementation according to the invention, the mobile system have stepper motor and especially along (or flat It is capable) (or being parallel to this) lead screw of track setting, the lead screw drives or can be driven by stepper motor.It can be made with this With conventional available component to realize the method and to realize the equipment.Stepper motor is configured to be directed to Property implement the movement stepping of definition, wherein the movement stepping includes being rotated with determining angular range.The step of stepper motor Into angular range that then can be determining corresponding to lead screw rotation, wherein the angular range is not necessarily equal to moved by motor The angular range implemented when one stepping.It is alternatively possible to which screw thread is arranged between stepper motor and lead screw.Another and lead screw The component of effect, such as rack rails can be implemented to move along path that is, especially straight line straight up when lead screw rotates Movement.The stepping of motor therefore can be equivalent to along lead screw definition move that is, what is defined moves distance or definition Mobile path length.Therefore the mobile path length of rack rails can be for example inferred based on the stepping-in amount of the motor monitored.Tooth Rail can for example make support system mobile or connect with support system.

In particular, the support system can have supporting member, heater is supported by the supporting member, and described Support system can have moving element, and the moving element is acted on lead screw in order to drive and especially guided by track. In addition, the support system can have force measuring device, support element is coupled via the force measuring device with moving element. In particular, the moving element may include rack rails, the rack rails acts on lead screw and converts the rotary motion of lead screw to Linear motion.Supporting member is not mechanically connected rigidly with moving element, via elastic element (for example including surveying in power Measure within device) connection.The measurement of movement routine indicates that the measurement of the position of movement routine and/or the parameter of length can be with It is related to the measurement of the parameter of supporting member and/or moving element.Moving element especially can be considered thus, because described Moving element primary (that is, directly passing through rigid mechanical element) is moved by means of motor.Supporting member only indirectly by means of Force measuring device and moving element are mobile.Therefore supporting member can flexibly be connect with moving element.If support system this Sample is constituted, then power measurement is also able to achieve other than traveling heater, so as to adjust the definition between orifice plate and container Pressing force, but avoid the damage or breaking-up of component simultaneously.

A kind of form of implementation according to the invention, the force measuring device include spring, the end peace of the spring Dress is on the mobile element and its another end is installed on supporting member；Grating (optoelectronic switch, Lichtschranke), It is coupled with stepper motor, wherein the spring compresses the distance of definition in the threshold value of power, thus triggers grating for mobile system It is placed in stopping.

The spring for example may include helical spring or leaf spring or these combination.The spring constitutes elasticity member Moving element is connect by part, the elastic element with supporting member.When heater has shifted to container, the edge in the gap of orifice plate The outer surface of the part below container can be touched first.The equipment make now heater together with the orifice plate of placement continue to Upper movement, so that the edge in the gap of orifice plate is with the higher and higher outer edge forced by container, therefore spring modification increases, is special It is not that compression increases.As spring-compressed increases, the cutting late (Schaltblech) of grating is close to each other and enough in compression Grating is interrupted when strong.The compression of spring, particularly compression distance can be connected by linear relationship (Hooke's law) with pressing force System or association.This can be determined by the indicatrix or calibration in advance of spring.It can interrupt when grating interrupts to step Into motor energy supply or optionally can be set brake.It can achieve the mesh at the final position of support system with this Cursor position or dbjective state.Fixation, such as magnetically fixed device or mechanical fastener, brake etc. are alsod relate to, with Just the state of pressing force reach in this way, required is kept.If system does not sound an alarm, can determine needed for presence The case where experimental condition wanted, gets off the test of execution standardization.

In a kind of alternative form of implementation, elastomer can be used as elastic element instead of spring.

In a kind of form of implementation according to the invention, the orifice plate and/or the container and following standardized assays at least One of be mutually compatible with: ASTM D86, ASTM D850, ASTM D1078 or ISO1078, these standardized assays respectively at least by The applying date effective version.

The orifice plate and/or the container can be mutually compatible with following specification or standardized assays in universal mode:

For the specification ASTM D86 of distillate fuel, 3405 ISO, IP 123, BS200-123, JIS K 2254, GOST 2177；

For the specification ASTM D1078 of solvent distillation, 195 IP, BS2000-195, ASTM D850, ISO 918, BS 4591,JIS K 0066,ISO 4626；And

Specification ASTM D524, IP14, BS2000-14, ISO of carbon residue are determined for providing bottoms 4262、ASTM D4530、ISO 10370。

A kind of form of implementation according to the invention provides a kind of liquid analysis system, particularly automatic distillation unit, with In the evaporation characteristic for determining liquid according at least one standardized assays, the liquid analysis system is included with opening, especially It is the container with the branch for leading to condenser；And the device for closed container, described device, which includes at least one, to be had The temperature measurement system of bar and temperature meter, particularly vapor (steam) temperature for measuring the liquid within container；With logical The closure member for closed container in hole, a part of the bar is directed across the through-hole in this way, so that temperature meter is set It sets within container；The supporting element that optionally there is the longitudinal direction on closure member transverse to bar to stretch out in closure member, institute Stating supporting element can push together with the counterpart of auxiliary device；According to described in one of above-mentioned form of implementation for preparing liquid Distill the equipment of measurement；And especially multiple standardized orifice plates, these orifice plates can be placed on heater.

The temperature measurement system can have one or more temperature meters, such as temperature meter, particularly Pt100 measuring appliance, the temperature, particularly holding that the temperature meter is structured in gas phase/steam phase of determining liquid At the position of determination within device.For this purpose, the vertical position of the first temperature meter can especially by thread mechanism energy Adjustment.Another second measuring appliance can be set for measuring the temperature on container bottom, do can for example to determine.

Vessel vapor can be sealed shut by the closure member, but support temperature measures simultaneously.It is described to hold for closing The device of device can also have analysis electronic device and electronic memory within the inner cavity limited by shell, so as to by one Or multiple temperature meters can store such as calibration data and/or to be able to achieve pretreatment to measurement data, for example to turn Change digital signal into.Furthermore, it is possible to communication interface is equipped among the electronic circuit within the inner cavity for closed device, with Just will especially digital measurement data wirelessly or wired connection be transferred on analytical unit outside.

Optional supporting element can keep when the device for closed container is pushed into vessel port and support whole A container.In particular, the supporting element can defined when the device for closed container is pushed completely into vessel port (especially vertical) position in keep the container.For the vertical position of the definition of container, for orifice plate and/or container Determine combination, can with movement routine/movement distance from previously known orifice plate to the mobile definition of container or definition it is predetermined The movement routine length of justice.If actual movable length is in advance not equal to this after heater is fully moved toward the bottom side of container Known movable length then it can be concluded that there is mistake equipment, such as has used vicious orifice plate and/or vicious appearance Device.It can be prompted to user, then user can replace orifice plate and/or container with correct component.

It should be understood that individually in any combination with for prepare liquid distillation measurement equipment it is associated or It is same as the feature that liquid analysis system is described, illustrates or provided with being associated can be according to the invention each in any combination Form of implementation is applied to the method for the distillation measurement for preparing liquid, and vice versa.

A kind of form of implementation according to the invention provides a kind of for preparing the method for the distillation measurement of liquid, the side Method includes: one orifice plate of selection from one group of standardized orifice plate；Orifice plate is placed on heater, the heater is configured to For heating container including liquid, being placed on orifice plate, determine that the evaporation of liquid is special to test for execution standardization Property；Keep heater (such as upward) mobile towards container；If the orifice plate being placed on heater reaches to the pressing force of container Threshold value then interrupts movement.

Detailed description of the invention

Each form of implementation of the invention is illustrated referring now to attached drawing.The present invention is not limited to shown or described realities Apply form.

Fig. 1 goes out liquid analysis system with schematic side illustration, and the liquid analysis system has according to the invention one The equipment of the distillation measurement for preparing liquid of a form of implementation；And

Fig. 2 schematically shows a kind of liquid analysis system of form of implementation according to the invention with side view.

Specific embodiment

Element with the same or similar structure and/or function passes through only different in first in different drawings Appended drawing reference indicate.To the explanation for the element being not described in detail in an attached drawing can from other accompanying drawings these are corresponding The explanation of element obtain.

Fig. 1 schematically describes a liquid analysis system 150, and the liquid analysis system has according to the invention one The equipment 100 of the distillation measurement for preparing liquid of kind form of implementation.Liquid analysis system 150 includes according to the invention one The equipment 100 of the distillation measurement for preparing liquid of kind form of implementation.The equipment 100 include heater 101, for example with The electric heater of heating solenoid, the orifice plate 103 selected from one group of standardized orifice plate can be placed into the heater On, especially on the upside of heater 101.In addition, for heating the container 105 being placed on orifice plate 103 comprising liquid Heater 101 be structured to execution standardization test to determine the evaporation characteristic of liquid.The liquid 107 to be studied, which is located at, to be held In device 105, it is configured to glass circle flask in container form of implementation shown in.

The equipment 100 further includes electrical mobile system 110, and the mobile system is configured to, and is used for heater 101 (especially together with orifice plate 103) 111 moves along vertical direction straight up and if is placed into the hole on heater 101 If the pressing force F of plate 103 towards container 105 reaches threshold value, the further movement of heating system is interrupted.

The container 105 is described to hold for closing at its upper end and by closing for the device 120 of closed container The device of device is only symbolically shown in Fig. 1.120 steam seal of described device closed container 105, particularly container it is upper It is open and can also be realized temperature measurement by means of at least one temperature meter 121, the temperature meter is arranged in bar 123 End on.The closure member 125 that the bar passes through described device 120 completely guides, wherein the closure member 125 is with outer surface It closely sticks on the inner surface of opening wall portion 127 of container 105.

Described device 120 further includes supporting element 129, and the supporting element dips down in side tiltedly to be stretched out and show with disconnection The counterpart 131 of auxiliary device out be connected, particularly form locking connect, to keep the device for closed container 120 together with container 105.

The mobile system 110 includes support system 133, and heater 101 is kept by the support system.The equipment 100 are structured to monitor and/or determine instruction along the length of the movement routine w of support system 133 and/or the ginseng of position z Amount.

The equipment 100 is also configured as the initial position za from support system that support system 133 is mobile straight To final position ze, at the final position, the pressing force F reaches threshold value.Support system is shown in FIG. 1 to be located at finally Pressing force F reaches the state of threshold value in the ze of position.In this state, the circular edge 135 of orifice plate 103 applies pressing force F Circular contact surface on to the outer surface of container 105 137.

At initial position za, the parameter that be arranged, instruction moves along the position in path has the first value, such as W1, and the parameter to the position of the instruction movement routine w of final position ze is arranged with second value, such as w2.The equipment 100 also set up the difference for the difference of the first value w1 and second value w2 to be calculated as to the movement routine length that instruction is passed through at this time w2-w1.Difference can for example be equal to or be equivalent to the amount of the stepping of stepper motor, between initial position za and final position ze The stepping have passed through by stepper motor.The type and/or parameter of orifice plate can be for example determined based on difference.

The support system 133 includes supporting member 139, and the heater 101 is supported by the supporting member.Bearing member Part is for example configured to platform and/or arm and/or bar, is suitably maintained or places having heaters 101 on it.Support system 133 further include moving element 141, and the moving element acts on to drive with lead screw 153, and the lead screw is set along track 143 It sets.In addition, the moving element is guided by the track 143 of along the vertical direction 111 orientations, movement routine w prolongs along the track It stretches.

Support system 133 further includes force measuring device 145, and supporting member 139 is via the force measuring device and mobile member Part 141 couples.Moving element is for example configured to moving arm or mobile station.Only moving element 141 is for example via rack rails and edge Vertical rail 143 or the lead screw being arranged in vertical rail 143 effect, rather than supporting member 139.Supporting member 139 and because This heater 101 makes 141 traveling time of moving element be grounded or secondary move by means of force measuring device 145 only secondaryly It is dynamic.

The force measuring device 145 have spring 147, an end of the spring be mounted in moving element 141 and Another end is mounted on supporting member 139.In addition, the force measuring device 145 includes grating 149, the grating and step It is coupled into motor 151, the stepper motor drives lead screw 153.If 147 boil down to of spring makes the threshold value for reaching pressing force F, The interruption element 155 of grating 149 interrupts the light beam 157 issued by light source 159, so as not to be detected by detector 161.Fig. 1 shows The state, mode are that interruption element 155 is arranged between light source 159 and detector 161 out, then manipulate motor 151 and stop Further movement.

The counterpart 131 of the support component 129 of the device 120 for closed container 105 may be mounted at track 143 Above or it may be mounted in other auxiliary devices.However, the machine of installation or fixation between counterpart 131 and track 143 Tool connection be advantageous, so as to container is placed in the definition relative to electrical mobile system 110 pre-determining position.

Fig. 2 schematically shows a kind of liquid analysis system 250 of form of implementation according to the invention, the fluid analysis System includes the equipment 200 for preparing the distillation measurement of liquid.

Liquid analysis system 250 shown in figure 2 has the similitude with liquid analysis system 150 shown in Fig. 1. Liquid analysis system 250 is especially configured to automatic distillation unit, for determining liquid according at least one standardized assays Evaporation characteristic, the liquid is located in container 205.Liquid analysis system 250 includes container 205, and the container has upper End is open and especially with the branch 263 for leading to condenser 269.It include to study in the container 205 Liquid 207.

The liquid analysis system 250 is also comprising the device 220 for closed container 205.The device 220 includes at least one A temperature measurement system, especially with the vapor (steam) temperature for measuring liquid within container 205, in inner cavity 264.In This, temperature measurement system includes the bar 223 on lower end with temperature meter 221, so that the temperature meter is arranged It adjusts or can adjust in this way in inner cavity 264 and especially along vertical height within container, so that the temperature meter It is located substantially in the height of branch 263, the branch leads to condenser 269, and the condenser is only symbolically shown.It is condensing The condensate generated in device 269 traps in trapping cylinder 271, wherein measurement trapping volume.

Described device 220 further includes the closure member 225 for closed container, wherein the closure member 225, which has, to be not shown Through-hole, a part of bar 223 is directed across the through-hole, thus temperature meter 221 be arranged within container, particularly Near branch 263.

Described device 220 further include on closure member 225 transverse to bar 223 longitudinal direction stretch out supporting element 229, The supporting element is pushed together with counterpart 231.In form of implementation shown in figure 2, the counterpart 231 and track 243 It is fixedly connected, movement routine w extends along the track, and heater 201 can be moved with orifice plate 203 along the movement routine together It is dynamic.

Therefore liquid analysis system 250 also includes the equipment 200 and especially multiple for preparing the distillation measurement of liquid Standardized orifice plate, the orifice plate can be placed on heater.Illustratively, the orifice plate in addition to being placed on heater 201 Other orifice plates 203b, c and d, the opening in the center that the orifice plate has parameter different or hole are also shown except 203a.

Mobile system 210 is equipped in order to make heater and orifice plate mobile (movement).Mobile system 210 includes stepper motor 251, the stepper motor keeps moving element 241 mobile, and the moving element is connect via spring 247 with supporting member 239.Bullet Spring and grating 249 are both the part of force measuring device 245, and the force measuring device is similar with being illustrated to reference Fig. 1 Function.The rotational motion of lead screw is changed into the linear motion for moving along path w by unshowned rack rails, and the lead screw is by step It is driven into motor 251.

Each form of implementation according to the invention provides a kind of method of automation, in the method user such as it is usual that Sample selects orifice plate, such as one of orifice plate 203a, 203b, 203c, 203d, these orifice plates are shown in FIG. 2.In next step In, it selected orifice plate is placed on heater 201 and is started automatically moves up.Here, heater with it is selected Orifice plate, such as 203a completely automatically push to or shift to flask or universal by lifter (mobile system 210 in other words) For on container 205.Once orifice plate is close on orifice plate, spring 247 compresses.If meeting or exceeding threshold value (this of spring force F Ground connection is determined via distance measurement using grating 249), then the movement of lifter or mobile system stops.Thus flask is avoided to damage It is bad.Meanwhile it being calculated by movement routine (that is, stepping of the stepper motor for example carried out till that time) in selected orifice plate The diameter in the hole within 203a and recognise that and selected correct orifice plate, so as to implement in advance as defined in standardization examination It tests.

Each form of implementation of liquid analysis system is configured to, according to specification ASTM D86, ASTM D850, D1078 or The test of 1078 execution standardization of ISO.In particular, these define four tools, there are four straight in different size of opening The orifice plate of diameter.Heater shifts to flask together with orifice plate from below.Here, orifice plate must be closed closely with flask.This ensures, with Heater is lightly pressed against flask.Here, existing in conventional device and method following dangerous, that is, damaged under excessive pressure Bad flask, such as glass rupture.If user or application person unintentionally select the orifice plate of mistake, do not allow to implement to test.

The temperature of steam (such as is shown in FIG. 2 in each form of implementation of the invention by means of Pt100 temperature sensor Sensor 221) measurement.Here, temperature sensor 221 is guided by bar 223 across closure member 225.In addition, holding for closing The device 220 of device includes another temperature meter 222, another described temperature meter other than temperature meter 221 Measure the temperature at container bottom, wherein another described temperature meter 222 passes measuring signal via another bar 224 It is sent in the inner cavity 226 within device 220, for example accommodates electronic circuit in the inner cavity, to handle measurement letter in advance Number and also in advance processing (first) temperature meter 221 measuring signal and especially implement calibration, and especially Digital signal can be converted to.Via being electrically connected between supporting member 229 and counterpart 231 not being shown specifically, especially Digital measuring signal is transmitted to the analytical unit not being shown specifically.For example may be used by means of another described temperature meter 222 With the determining point done that is, the last remnants of liquid evaporate within container, because in this case on container bottom Temperature improves strongly.

Each form of implementation of the invention be also able to achieve avoid operating mistake and especially starting distillation measurement before by According to standardization experimental examination, if always used and accordingly met orifice plate specification and compatible with selected test.

Form of implementation according to the invention, user thus can in the unit of automation according to fluid sample and/or Distillation sequence selects four by one of orifice plate of specification defined and also selects affiliated flask or container and start measurement. Then lifter guides orifice plate from below to flask and the orifice plate with forcing of defining is close to flask, so as to accurately close Joint seal gap.

Container 105 and the orifice plate 103 on heater 101 compress relative to one another.For this purpose, lifter (or bearing member Part 139) moved by stepper motor 151, the stepper motor by wire thilling driver 153 make the receiving portion of heater 101 along Guide rail 143 moves.Final switch is located at two terminal points, so that movement routine/movement road of lifter be clearly defined Journey.Movement routine/movement distance resolution ratio is determined by the pitch of step resolution and lead screw.Power is measured by means of spring 147 and with cutting door screen 155 grating 149 carry out.Stopping of the lifter in determining power is normal by spring with definition The compression of several springs and carry out.According to Hooke's law (F=Dx Δ L) in fixed spring constant D (such as 0.5N/mm) length The compression of Δ L (such as 5mm) exactly corresponds to power F.Stop being carried out by means of the grating triggered according to length Δ L, so that it is guaranteed that Heater is pressed on flask with the power F of definition.If therefore orifice plate guides flask into from below, (measured by distance Δ L ) spring force raising.If it exceeds the threshold, then moving stopping.By means of stepper motor until the amount for the stepping passed through at that time Infer bore dia or corresponding orifice plate.

Illustratively, following table 1 for different determinations movement routine/movement distance show to this corresponding flask with The combination of orifice plate.

Table 1:

Flask	Orifice plate	Mobile distance
			125ml	50	28mm
125ml	38	25mm
			125ml	32	23mm
125ml	25	20mm
			200ml	50	38mm
200ml	38	35mm
			200ml	32	33mm
200ml	25	30mm

Tolerance or the +/- 1mm of precision are applicable in respectively for the mobile distance being given in Table 1.By adjusting specification, user It can check, the whether selected orifice plate and correct flask according to specification of user.If user has selected the hole of mistake Alarm or the audible signal that can sound, then can occur over the display in the flask of plate or mistake.When necessary, if be not used Correct component can then require user to replace orifice plate and/or flask or interrupt start distillation measurement.