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CA1122443A - ANALYSIS CELL FOR FEEDING .alpha. DIKETONES FOR THEIR MEASUREMENT UNDER CONTINUOUS FLOW CONDITIONS - Google Patents

ANALYSIS CELL FOR FEEDING .alpha. DIKETONES FOR THEIR MEASUREMENT UNDER CONTINUOUS FLOW CONDITIONS

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Publication number
CA1122443A
CA1122443A CA319,262A CA319262A CA1122443A CA 1122443 A CA1122443 A CA 1122443A CA 319262 A CA319262 A CA 319262A CA 1122443 A CA1122443 A CA 1122443A
Authority
CA
Canada
Prior art keywords
product
feeding
cell
path
injector
Prior art date
Legal status (The legal status 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 status listed.)
Expired
Application number
CA319,262A
Other languages
French (fr)
Inventor
Gilbert Bauer
Remy Roth
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
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.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Application granted granted Critical
Publication of CA1122443A publication Critical patent/CA1122443A/en
Expired legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02Food
    • G01N33/14Beverages
    • G01N33/146Beverages containing alcohol

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Apparatus Associated With Microorganisms And Enzymes (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)

Abstract

ABSTRACT

An analysis cell for feeding ? diketones for their measurement under continuous flow conditions has a feedpath and a reference or blank path. Each path comprises in series, an injector for introducing reactant and air into a solution of distillation condensates from the sample, a mixing coil, a delay coil, an acid injector, two mixing coils, a debubbler, an air injector, and if required a supplementary debubbler. This invention is of use in industries producing fermented products, fermented drinks, and in particular beer.

Description

2;2 9L43 This invention relates -to an analysis cell for feeding ~ diketones and their precursors under con-tinuous flow conditions, Por their spectrographic determination in a liquid or extract, and in particular~
in beer during the fermentation stage, in the finished beer or in the wort.
~ he automatic control of a fermentation process requires a precise knowledge at all time, or at least at close time intervals~ not only of the values of the parameters which are characteristic o~ its proper progress, but also of the value of the variables which in~luence the quality of the final product.
This is notably the case in beer fermentation, during which the value of the concentration of ~
diketones, and in particular ace-tyl and 2-3 pentanedione a and their respective precursors, c~ ace-tolacetate and c~
acetohydroxy~u-tyrate9 indicate the stage which the process has attained. If the fermentation is properly controlled, then this concentration notably passes through a maximum during the active fe~mentation stage, and diminishes to fall to a low value.
IP the changes in these concentrations drift outside an estimated normal rangeJ the process gives rise to a poor quality product. Thus, the persistence in the final product o~ ~ diketones, in particular diacetyl, and their pre-cursors is one o~ the main reasons for the wrong taste in beer.
~t has been noted that if the yeast works properly, then the diacety~ content ~alls suddenly at the end of Eermentation.
. This sudden change inveriahl~ indicates the termination of the process if it has taken place under proper conditions, and can serve as the control signal for the cooling which constitutes the stage following fermentation.
An object of the invention is to feed ~ diketones and their precursors under continuous flow conditions by pro-viding an analysis cell to be located within a continuous flow measuring network in which the determination is made by spec-trophotometry.
~ ccording to one aspect of this invention there is pro-vided an analysis cell for incorporating within a continuous flow measuring network, for feeding ~ diketones, and their precursors for the determination of their concentration by spectrophotometry, using distillation condensates from a sample of liquid or extract, comprising a feed path and a reference path, each path comprising an inlet in the form of three conduits, for air, for the product to be fed and for a reactant, and which lead to an injector, and each path continuing in order, through a homogenisation coil, a delay coil, an injector for a hydro-chloric acid eed circuit, at least one homogenisa-tion coil, a free flow conduit, a debubbler, a conduit passing through a pump, an air injector and a conduit for supplying the measuring :~strument.
The cell according to -the in~en-tion represents subs-tantial progress in determining c~ diketones and their precursors. It also gives indispu-table and importa~t advantages.
Firstly, it enables spectropho-tometric determination under continuous flow conditions of the c~ diketone content ~hen used to complete this type of measurlng network.
It consequently allows constant monitoring of the changes in its concentration, and can use -these determina-tions to control the corrections to be made.
In particular, it makes it possible to control the latter stages of the process and their initia-tion~ in par-ticular the cooling stage after the actual fermentation.
It ensures that two samples are to-tally independent by preventing contamination at any level. Because of this, several fermen-tation vats can be investigated successively.
Acco~ding to another aspect o~ this invention -there is provided a process for feeding ~ diketones and their precursors contained for determining their concentration under continuous flow conditions by spectrophotometric measurement, comprising isolating -the volatiles by distillation7 feeding an alcoholic solution of the con-3L9 ~ 3 densates, together ~ith a wetting agent into a cell,bringing said solution into contact with a reactant, namely, orthophenyldiamine as a 1% acid solution in 4N
hydrochloric acid, simultaneously segmenting said solution into elemtary samples separated by air bubbles, mixing the product, delaying the product so that the reaction can be completed, injecting a 4N hydrochloric acid solution into -the mixture, homogenîsing the resultant product, passing the product ~hrough a conduit which does not pass throug~ a pump, restoring continuous flow conditlons, passing the product -through the pump, segmen-ting the product, and feeding the samples in-to a measuring instrument An embodiment of the invention will now be described, b~ way of example with refere~ce to the drawings:-Figures la and lb are block dlagrams of the two pathsof the cell, namely, the feed path and the reference or blank path respectively.
As stated, the invention provides an analysis cell 2.0 to be located within a con-tinuous flow measuring network~
comprising an assembly of circuits for feedingc~ dike-tones, in particular diacetyl, and their precursors for the purpose of de-termining -their concentration by spectrophoto-metry after their isolation from a sample of liquid or extract? for exampleJ beer during fermentation.
The cell accordi~g to the invention comprises a feed 4~

path 1 for measurement purposes and a reference or blank path 2 which enables the measurements to be made free of any parasitic variation or interference. This neutral path is made iden-tical to the feed path in its composition and arrangement, so as to undergo the same in~luences and parasitic variations.
The product to be fed is replaced in this reference or blank path by an alcohol solutlon7 for example a 10%
solution, and which is a function of the alcohol content of the product to be fed for measurement purposes, -together with 0.5 ml of a wetting agent.
The cell is composed of conduits in the form of glass tubes which convey the mixtures and thelr various additives.
Practically all the circuits which make up the reference and measurement paths pass through -the pump of the continuous flow measurement network.
The various f-ow rates in the air7 reactant and acid conduits are adjusted to ob-tain proper hydraulic operation of the assembly~ Thus, the conduits are made up by adapting gauged tubes.
Entry is through three different conduits, a first conduit 3 for air, and a second conduit 4 for the product to be fed~ This is in the form of condensates from the distillation of the actual sample dissolved in alcohol to an extent which is a function of the alcohol contained in the sample, for example 5%, toge-ther with a wetting agent.

a43 This latter ensures proper hydraulic operation, and prevents contamination between severl elementary samples separated from each other by an air bubble.
This is because the wetting agent facilitates progression without jerks, i.e. a regular flow. It also means that the sample does not leave traces on the walls.
The las-t conduit 5 carries a reactant, namely orthophenyldiamine, for example in a concentration of 1%
in a 4N hydrochloric acid solution in the case of beer.
These conduits lead to an injector 6 where the distillation samples are brough-t into contact with the reactant, and segmen-tation takes place by interposing air bubbles.
The circuit continues through a homogenisation coil 7, for example, comprising five turns, where actual mixing takes place be~ore passing through a delay coil 8 for holding up and completing the reaction.
At its outlet, there is an injector 9 connected to a circuit 10 for feeding 4N hydrochloric acid~ The circuit then continues through two homogenisation coils~
11 and 12 having similar characteristics and each posses-sing at least fourteen turns, and then emerges through a circuit 13 which does not pass through the pump, i.e. i-t flows freely into a debubbler 149 the surplus ~rom which is fed to drain at 15.
Con-tinuous flow is provided downstream through the ~Z~3 circuit portion 16 in order -to ensure proper hydraulic operation of thè assembly, after which it is re-segmented into elementary samples by an injector 17 fed with air through the conduit 18.
In this way, by re-segmenting the flow and again passing it through the pump, a regular flow can be obtained at -the inlet to the spectrophotometer.
The circuit proceeds via a portion 19 which leads to a final debubbler 20, the discharge 21 from which is fed to drain and the outlet 22 of which is connected to the container of the measuring instrument.
In the case of spectrophotometers with an incorpora-ted debubbler, this debubbler would form part of the instrument itself.
The sample is returned after measurement and then discharged by an auxiliary circuit 23 which passes through the continuous flow pump.
Thus, the withdrawn and distilled samples are broken down into elementary quantitites isolated by bubbles, described heretofore as elementary samples, in order to prevent any contaminations. In addition, for hydraulic reasons, continuous flow is recreated in two stages within the cell.
As indicated, the reference path 2 is composed of the same members arranged in the same manner. These are consequently given the same reference numerals but with ~ 2'24~3 lef~r a the ~*~er added.
The following operations are carried out in the analysis cell according to -the invention in feeding elementary samples under con-tinuous flow conditions prior to their measurement.
The phase to be measured is previously isolated ~rom the ~ithdrawn sample by distilla-tion and condensation.
The condensates are conveyed to the inlet of the cell in an alcoholic solution which is a function of the acohol quantity in the condensate, for example 5%, together with a wetting agent.
This solution is taken and brought into contact with a reactant, Ilamely orthophenyldiamine in the form of a 1% acid solution in 4N hydrochloric acid, and is segmented into elementary samples separated by air bubbles, by means of the injectors.
The products are then fed through the homogenisation coil 7 and traverse the delay coil 8 for holding up and completing -the reaction with the reagent.
A 4N hydrochloric acid solution is injected down-stream into said mixture through the injector 9.
The resultant product is then homogenised through the -two successive coils ll and 12 each comprising a large number of turns.
The product is then passed through the conduit 13 which does not pass through the pump of the continuous flow network.
At the outlet, it is passed through the debubbler 14 in order to return it to continuous flow.
The product is passed through a co~duit which passes through the pump~ as in the case of all the others, and it is again segmented by the injector 17.
It then passes through the debubbler 20 to provide a continuous feed to the container of the spectrophotometry instrumentl I0 If this latter possesses an incorporated debubbler, the feed is made directly.
Exactly the same operations are carried out in the case of the reference or blank path 2, by ~eeding the sample path with an alcoholic solution which is a ~unction of the alcohol content of the condensate, for example 10%
.
in the case of a sample of fermenting beer, together with a wetting agent.
Although the invention has been described for a determined application, namely to provide a feed for the continuou~ measurement o~ c~ diketones contained in a sample o~ ferme~ting beer, other similar applications fall within its scope.

Claims (6)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED APE DEFINED AS FOLLOWS;
1, An analysis cell for incorporating within a contin-uous flow measuring network, for feeding .alpha. diketones, and their precursors for the determination of their concentration by spectophotometry, using distillation condensates from a sample of liquid or extract, comprising a feed path and a reference path, each path comprising an inlet in the form of three conduits, for air, for the product to be fed and for a reactant, and which lead to an injector, and each path continuing in order, through a homogenisation coil, a delay coil, an injector for a hydro-chloric acid feed circuit, at least one homogenisation coil, a free flow conduit, a debubbler, a conduit passing through a pump, an air injector and a conduit for supplying the measuring instrument.
2. An analysis cell as claimed in claim 1, wherein each path comprises a further debubbler.
3. A cell as claimed in claim 1, wherein the reactant is orthophenyldiamine as a 1% concentration in a 4N acid solu-tion.
4. A cell as claimed in claim 2, wherein the reactant is orthophenyldiamine as a 1% concentration in a 4N acid solution.
5. A cell as claimed in claim 1 wherein the injectors provide segmentation into elementary samples separated by air bubbles.
6. A process for feeding ? diketones, and their precursors contained for determining their concentration under continuous flow conditions by spectrophotometric measurement, comprising isolating the volatiles by distillation, feeding an alcoholic solution of the condensates, together with a wetting agent into a cell, bringing said solution into contact with a reactant, namely, orthophenyldiamine as a 1% acid solution in 4N
hydrochloric acid, simultaneously segmenting said solution into elementary samples separated by air bubbles, mixing the product, delaying the product so that the reaction can be completed, injecting a 4N hydrochloric acid solution into the mixture, homogenising the resultant product, passing the product through a conduit which does not pass through a pump, restoring continuous flow conditions, passing the product through a pump, segmen-ting the product, and feeding the samples into a measuring instrument.
CA319,262A 1978-01-30 1979-01-08 ANALYSIS CELL FOR FEEDING .alpha. DIKETONES FOR THEIR MEASUREMENT UNDER CONTINUOUS FLOW CONDITIONS Expired CA1122443A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR7803284A FR2415802A1 (en) 1978-01-30 1978-01-30 ANALYTICAL CASSETTE FOR THE DETERMINATION OF ALPHA-DICETONES AND THEIR PRECUSERS
FR78/03284 1978-01-30

Publications (1)

Publication Number Publication Date
CA1122443A true CA1122443A (en) 1982-04-27

Family

ID=9204250

Family Applications (1)

Application Number Title Priority Date Filing Date
CA319,262A Expired CA1122443A (en) 1978-01-30 1979-01-08 ANALYSIS CELL FOR FEEDING .alpha. DIKETONES FOR THEIR MEASUREMENT UNDER CONTINUOUS FLOW CONDITIONS

Country Status (9)

Country Link
JP (1) JPS54113396A (en)
BE (1) BE872349A (en)
CA (1) CA1122443A (en)
CH (1) CH633111A5 (en)
DE (1) DE2852467A1 (en)
FR (1) FR2415802A1 (en)
GB (1) GB2013336B (en)
LU (1) LU80524A1 (en)
NL (1) NL7811390A (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01182752A (en) * 1988-01-14 1989-07-20 Chugoku Shoyu Jozo Kyodo Kumiai Continuous turbidity measuring method in manufacture of potable liquid
DE4002108A1 (en) * 1990-01-25 1991-08-01 Tuchenhagen Otto Gmbh Testing of beer mash strength and sugar content and appts. - by extracting mash from stream and mixing in given ratio with iodine soln. before continuous measurement in optical measuring tube
GB9201568D0 (en) * 1992-01-24 1992-03-11 Honeybourne Colin L Food spoilage detection method
JPH05240838A (en) * 1992-02-27 1993-09-21 Kagome Co Ltd Method for measuring diacetyl contained in processed food and drink
DE102017220514A1 (en) * 2017-11-16 2019-05-16 Unisensor Sensorsysteme Gmbh Method and device for detecting foreign substances in a liquid medium

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4025311A (en) * 1976-01-09 1977-05-24 Bochinski Julius H Programmed fluid sampling and analysis apparatus

Also Published As

Publication number Publication date
LU80524A1 (en) 1979-03-22
CH633111A5 (en) 1982-11-15
GB2013336B (en) 1982-12-01
FR2415802B1 (en) 1981-06-26
NL7811390A (en) 1979-08-01
FR2415802A1 (en) 1979-08-24
JPS54113396A (en) 1979-09-04
DE2852467A1 (en) 1979-08-02
BE872349A (en) 1979-03-16
GB2013336A (en) 1979-08-08

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