CA2253354A1 - Process and device for determining the oxidisable substance content of aqueous liquids - Google Patents
Process and device for determining the oxidisable substance content of aqueous liquids Download PDFInfo
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- CA2253354A1 CA2253354A1 CA002253354A CA2253354A CA2253354A1 CA 2253354 A1 CA2253354 A1 CA 2253354A1 CA 002253354 A CA002253354 A CA 002253354A CA 2253354 A CA2253354 A CA 2253354A CA 2253354 A1 CA2253354 A1 CA 2253354A1
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- 239000007788 liquid Substances 0.000 title claims abstract description 21
- 239000000126 substance Substances 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title claims description 13
- 239000007789 gas Substances 0.000 claims abstract description 21
- 238000002485 combustion reaction Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 4
- 239000002912 waste gas Substances 0.000 claims 2
- 230000008020 evaporation Effects 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 101100536354 Drosophila melanogaster tant gene Proteins 0.000 description 1
- 101150052091 Sarnp gene Proteins 0.000 description 1
- 108020004566 Transfer RNA Proteins 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012476 oxidizable substance Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1826—Organic contamination in water
- G01N33/1846—Total carbon analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1886—Water using probes, e.g. submersible probes, buoys
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/06—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by combustion alone
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Combustion & Propulsion (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
To determine the oxidisable substance content of aqueous liquids, a sample chamber (1) is filled with the liquid and emptied again, a small quantity of the sample remaining on a heating element (10) projecting into the sample chamber (1). With the sample chamber closed, the heating element is briefly heated, whereupon the adhering quantity of sample evaporates and the oxidisable substances are burnt. The pressure or moisture increase thereby occurring is used to determine the quantity of the sample. The quantity of exhaust gas produced by combustion is found by infra-red measurement and the oxidisable substance content, especially carbon or nitrogen, is found from both values (quantity of sample, and quantity of exhaust gas).
Description
l ~U ~U WLIJ 1~ II CA 022~33~4 1998-10-27 1 I~)J ~JJ~ ~U~l ~ U
FILF ~1 ~ S Altlr~
1*~ ~, ','~r~L~'~'li';' Proce~s and device for the dete~rnination Df the content of oxidzable su~ ~s in a~ueous liquids.
l'he in~rention relates to a ~ c~ss for the det~ n of the co-~tf-~t of oxidizable substi~n~e~ in a~lueous liqu~ds, iXI vJhich liquid s~slples are 1esd to a cc)mbustion fi~nace and are t~ermally treakd~ and tha substance i5 burned to a ,gaseous oxide ~nd, in a sample of the wast~ gas thus obt~ined, the contc,~t of the ~asev~ o~ide is detc.n~;~.cd b~ means of ir~frared measurement.
An i~,~o~ td~t area of use of this process is the deti. f~ .ir.~tion of the carb~n ~Ullt.,~lt and~or o:f the rlitrogen conte~t in ef~luent. These oxidizable sut stPnc~s are gcnera~ly lc r~ d to as follo~s.
TC (Total Ca~bon) the total value of the carbon contained in the a~ eous li~uid;roc~ (Total Organic C~a~bon) the total carbon contnined in the fo~m of'organic compounds in the aqueous liquid;
T~C (Tot~I Inor,ga~i~ Carbon) the total carbo~ eQrtSIin~A in the form of inorganic compounds in the aqueous liquid;
T~l (Total Nitrogen) the total r~ gen co..~u~d in the aqucous liquid.
In the essay by ~. Ehrenb~rger, "~or the Detennin~ti--n of Oxygen Dem~nd- and Carboll Idcntification ~l~nbers in the I~et~rrnin~ti~n of Watex Quality," GIT ~achz. I~ab. vol~ 23, ~u~. 1979, pp. 738--74~, desc2ibed are various methods for the TOCI~t~ ation, W71ich methods are bas~d on the wet-chernical and tt~ re~ion of organic s~ ces and the q~antitat~ve ox~d~tion.
~n the ~cnown ~r~cesses of the type men~ioncd initially, the liqu~d sample n~ns d~rnu~
oil filter to remove particles that are larger th~ 10~200 unt. l he liquid sample wa~ then --in the case of the d~t~ ;o~ of dle TOC optionall~r w~th an inte~ediate tl r,A ~ r.
for the rcrl~oval of the inorganic compo~ulds lead to tbe combustion furnace. 'rhere the olganic su~k.:~lces are rh~ally converted to carbon dioxide (Co7). The carbon dioxidc .u ~ J~ "" u~ CA 02253354 1998-10-27 1 ~u~ UJ~ ~U~
ob~ained is transported by me;~ns of a ~ olt~ fhich usually also delivers the n~C~s~r combu~ion ox~gen, through a coole~ ~i~ a wate~ s~ tor, a gas filter and an i~ed analyz~r. ~hc carbon dioxide o~n~ed dunng the comb~stion is determined through in~a~ed mea~uremeJIt, arld from dlis val~le ~e TO~ is calcu1~
Ix~ the described process, the sample volume pe~ unit of ~ime o~ single sample w~th 20-100 micro liters is ex~emely small. The small sample volunle resllIts in that the lines that lead to it also have to have ex:tremely small cross-sections, to avoid lar~e~ losses of time.
A fur~e~ knoun process ~wf-wa~er/~ffluent 120 ~1979) H. 5] for the ~OC-de~r-ni..ation ~vithout the use of ~ catalyst requires hi~her t.,.n~at-lres (110~l200~C) a~d a lon~er lenc,th of stay in the fumace. A simple pr~lon~ing of the le~xth of stay in the ~nace through enlargement ofthe furnace voIume, however has ~:he disadvanta~e o~lollger dead times. The same effect is stri.ven for in ~e kno~rn process in that thc sarnp~es ~aixed witb a carrier ~as are lead, on their way through the corn~ tion fi~m~ce, thro~gh t~e hottest furr~ce zones by means of nnetal sheets to change theLr d~rection ~disturbances), prior to Icaving the fumace, and are lcad to th~ ar~t messutement for ana~ysis.
The sample is placed into the furnace by mea~s of a lr~ns~l gas (c~rrier gas) and/o~
micro-nozzle dosing device. I~ doin~ so, the following contcxt is impo~tant:
The sarnple ~olume, ha~ng 2~100 micro 1iters, is ~ clr small It has to be injected i~to ~he combus~ion fLlmace alo~g ~~rith a carrier gas. llle carrier ga~ has ~e main function to transport ~e C~02-gas d~at has been obtained ~ough ~e combustion oue of the combustion fi~r~ace to an m~ared mea~ ment chamber. The an~o~mt of c~r~ie~ gas deterrnines the time period of the COZ exchasl~e in ~e combustion furnace. The amo~nt of thc carricr gas, h~wever, dilutes the product si~nal of t~e COZ to be measured ~rom whioh the TC, TOC etc are deteIminet.
In order to achieve a good entry of the effluent into the con~ Aon fumace given the aforementionet corlditions, a rne~nir.~l device has to t~yO~t ff~e samp~e with a high ~J~JI CU J~J ~LLJ I I ~)J 1111 L~ Il CA 022~33~4 199X-10-27 1 IJ~ ~U~ IV
.. . . . . .
ellergy ~ough a very ~hin noz~le into the combustion fiumace, or the liquid sa~ple has t~
be injected into the co~bustian furnace vvi~ the help of the c~r~e~ gas throug~L a lrex~r thi~l no~le (a nozzle with a v~ry s~nall cmss-section).
The ~ecess~ry obse~v~nce of t~e above~ "ltioned COII~itiOllS results in that the L~se of ti~e injection no~zles with a very sma~ tçr (5(~250 llm) very quicl~ly leads to the clo~ging up of the ~oz~te. If the nozle is enlarged, more calTier ~as has to be employed Ln orde~ to ~ozzle the mixnlre in the combustion film~ce with enouE~h enetg~r. In so doing, the product signal of the ~O~ is rcduced It is the~efore the object of t~e invention to arr~nge a process of the initially men~l~ned typc in such a w~y that, ill a s~mple vvay, a vely small ~ut very exactly determinable sample amount can be introduced intn the combus~ion fumace without that, in dou~g so, a ca~ier gas is u~ed a~d/or that the d~nger of the clogging of ~he thin lines e~ists l~e problem i~ solved according to the invention in that a liquid s~ ple h~n~ine onto a heating sur~ace is evapo~ated du~ing, a closed combustion fumace i~ order to ~ tS ;- \ the waste ~as sanlple to be lead to tl~e i~ d measu~ement, and ill that ~he pressure inc~ease in the combustion fu~nace ~enerated dur~ng the evapora~on or the humidity increase in the gas is meas~red ~nd, based on it, the sarnple an~ount is calculated.
In so doin~3, the separation of a ve~y small amount of sample occurs sunply for the reason that the ~mount of liquid that remains on ~he he~mg su~ace aI~ter the wctting of the heat~ surface with the li~uid ~onns the desired srna~l sample al lou~t, of wh~ch the voll~ne still has to be exac~ly doterrmned. This deternlination of Ihe vo1ume is conducted in a very sLmple n~ r~; ~rith high accuracy in that the ~l~iS~u~, increa~e that i~ cl ~Icd in the evaporntion or t~e humidity i~ c is measured. Tbis incr~ in the p~essure ~
case in the humidity can be lead m~ ically ba~ to thc e~ dted ~ou~t of the liquid.
In an especia~ly simple m~nn~r, ~e we~ting of the heat~Lg surface occurs in that th~
con~bustion furnace is at least partially filled with the Iiguid to bc ~ y~ed and iS then ~ . ~ . . . ~, .
~ U ~ h~J 11~ 1111 ~V~II CA 022~3354 1998-10-27 ~ UJU ~UCI I . ~
emp~ied throu~h the addition of gas The fnct that also the walls ~f ~e combustion furnace ~re ~ve~ed with the liquid does not mflllence the l,lea~u.~...en~ results bee~c the amount of the liquid h~neit~ on the ~alls is n~t ~.f..por~ted asld is thus nut considered i~
the analysi~.
~ device accordJn~ to the inve~tion for conducting the ~rocess that has a combustion furnace and a con~ectt~d device for infra~d meas.lr~lue,~lt is characterizcd in that the combus~o~ furnace h~s a fi~rnace C~A~ at can be closed, in which a h~ting eleme~t extends up~ard, and ~o ~hich a p~esslJre measuring device is at~ached.
Further adva~ta~geous embodiments of the spLnt of t}le invention are the obj~ct of fi~ er dependent claims.
In the ~ollowing, an example of an enlbotiment of the i~vention is de~c~ibet in det;ail as show~ in ~e diAgra~n.
The diagram shows, ih a ~imp~ified longitudi~al cr~o.s-~eclion, a device f~ the deterrnination of the C~llte"lt o~' o~idizable su~sl ~nees in aqueous liquids, especially the conte~t of carbon or nitrogen in e~ . ~ samp1e chamber I is a~ ,e~ in a me~uringb~oy 2 to be imm~ sed into the effluent to be analyzed. On the floor 3 of the chamber, a ch~mber open~ng S is arranged that can be closed usi~ a valve 4. Throu~h ~ ~s i~let valve 6 and a gas line 7 ~at extends upward fr~m the sample chamber 1, oxygen o~ (~o2_ free gas c~ be lead. As a 1pres~.ure l~leastllulg device, provided is a p~e~ mea~unng capsule 8 as ~ ed to the sample chamber 1. InYtead of this, also ~ humidity-measuring device can be provided. A gas-~elease valve Y serves to rele~se the g~ls fiom the ~.ample chamber 1. A~ a hes~ng element, a ~lowin~ wire 10 extends firom the sarnple chamber 1.
A dosing device 11 for the a~ldition of acid to chan~e the pH value is co~ected to the ssnlple chamber 1.
I~he sample chamber I which senre~ ~s reaction chaxnber or cornbustion filrnace is filled~
vl~en the valve 4 is opened and the gas-release valve 9 is open. with ~e cPfll~e~t ~o be ~ L~
~v ~ u ~ v ~1~1 .,., ~1, CA 0 2 2 5 3 3 5 4 19 9 8 - 10 - 2 7 ~ U ~, u . ~
.. . . . .................. _ . ..... . . ... ..
analyzed which flows through ~e charnber op~n-ng 5 illto the sample r~rnb~r 1 bymeans of the hydrostatic pressure of the ef~luent surroundin~ the n~ . ;n~ buoy 2. I hen the valve 4 is elosed. ~Jpon use of a p~-me~suring dcvice, a pH-value of, ~or example, 2-3 is set ~rou~h the addition of acid via a dosing device I I . The~ e s~nple ch~nber I is gassed via ~ gas-i~let ~ralve 6.
By mcans of the l~cnvt,~tu~g gas, dle ~1vater cQ~t~ined in the samplc chamber 1 is pushed out through the chamber opening 5 while the valve 4 is open. Then the val~e 4 on the charxlber floo~ 3 and the ~ in1et valve 6 are closed.
The he~ing element l O is we~ted ~vith a small anlount of the effluent to be analyzed. ~he heating element 10 is heated to l O00 120(~C for a short period of time. ~n so doing, the w~ter t~lat is adhering to the heatin~ element 10 is in.~t,..~ne~.usly evapotated arld increases the prcss~lre in the sample chamber l. l~merli~t~ly thereafter, the oxidizable substances contained in the w~te~ are burned to Co2 alld ~JO.
I~e pressure increase that is ge~erated by the e~a~ol~ali~ is ~neasured irl the pressure-measuring capsule 8 Instead o~this, al~o ~e h.~ ty inclcdse in the ga~ carl be mea~ured. From ~is~ the a~ ullt of the evaporated water is de~in~ n an ar~ly~er (not showxl he~e).
By opening the gas-inlet valve fi and the gas-release ~alve 9, the y,~ e~ l combus~on gas CO~ andJor NO are lead to a device (not shown here) fo~ the in~ared rneas~GI~c~t and a~e me~sured. rl~e value thus obtained equals, together w~th the amo~t of t~e evdpGr~d sample of wbich the volume has been determined from the pressure i~c.~eor fiom the hu~nidi~ increa~e, the content of oxidi~able substances, La the described example the content of c~rbon and/or nitrogen.
The ~rocess was described usin~ the e~mple of a n~e&~ing buoy immersed into thc ef~uent. ~t is ~mde~stood t}lat the process can also be adv~nta~eously enlployed in another ~5' ~JUI ~U UU ~ II'UU 1111 U~ I CA 02253354 1998-10-27 ' ~UJ U.1~J ~U~I ~, VU, IU
embodiment of the device, for exa~nple, when the ef~uent to be analyzed cont~ined in ~e sample ch~rnber is supplied via a line and a pump.
FILF ~1 ~ S Altlr~
1*~ ~, ','~r~L~'~'li';' Proce~s and device for the dete~rnination Df the content of oxidzable su~ ~s in a~ueous liquids.
l'he in~rention relates to a ~ c~ss for the det~ n of the co-~tf-~t of oxidizable substi~n~e~ in a~lueous liqu~ds, iXI vJhich liquid s~slples are 1esd to a cc)mbustion fi~nace and are t~ermally treakd~ and tha substance i5 burned to a ,gaseous oxide ~nd, in a sample of the wast~ gas thus obt~ined, the contc,~t of the ~asev~ o~ide is detc.n~;~.cd b~ means of ir~frared measurement.
An i~,~o~ td~t area of use of this process is the deti. f~ .ir.~tion of the carb~n ~Ullt.,~lt and~or o:f the rlitrogen conte~t in ef~luent. These oxidizable sut stPnc~s are gcnera~ly lc r~ d to as follo~s.
TC (Total Ca~bon) the total value of the carbon contained in the a~ eous li~uid;roc~ (Total Organic C~a~bon) the total carbon contnined in the fo~m of'organic compounds in the aqueous liquid;
T~C (Tot~I Inor,ga~i~ Carbon) the total carbo~ eQrtSIin~A in the form of inorganic compounds in the aqueous liquid;
T~l (Total Nitrogen) the total r~ gen co..~u~d in the aqucous liquid.
In the essay by ~. Ehrenb~rger, "~or the Detennin~ti--n of Oxygen Dem~nd- and Carboll Idcntification ~l~nbers in the I~et~rrnin~ti~n of Watex Quality," GIT ~achz. I~ab. vol~ 23, ~u~. 1979, pp. 738--74~, desc2ibed are various methods for the TOCI~t~ ation, W71ich methods are bas~d on the wet-chernical and tt~ re~ion of organic s~ ces and the q~antitat~ve ox~d~tion.
~n the ~cnown ~r~cesses of the type men~ioncd initially, the liqu~d sample n~ns d~rnu~
oil filter to remove particles that are larger th~ 10~200 unt. l he liquid sample wa~ then --in the case of the d~t~ ;o~ of dle TOC optionall~r w~th an inte~ediate tl r,A ~ r.
for the rcrl~oval of the inorganic compo~ulds lead to tbe combustion furnace. 'rhere the olganic su~k.:~lces are rh~ally converted to carbon dioxide (Co7). The carbon dioxidc .u ~ J~ "" u~ CA 02253354 1998-10-27 1 ~u~ UJ~ ~U~
ob~ained is transported by me;~ns of a ~ olt~ fhich usually also delivers the n~C~s~r combu~ion ox~gen, through a coole~ ~i~ a wate~ s~ tor, a gas filter and an i~ed analyz~r. ~hc carbon dioxide o~n~ed dunng the comb~stion is determined through in~a~ed mea~uremeJIt, arld from dlis val~le ~e TO~ is calcu1~
Ix~ the described process, the sample volume pe~ unit of ~ime o~ single sample w~th 20-100 micro liters is ex~emely small. The small sample volunle resllIts in that the lines that lead to it also have to have ex:tremely small cross-sections, to avoid lar~e~ losses of time.
A fur~e~ knoun process ~wf-wa~er/~ffluent 120 ~1979) H. 5] for the ~OC-de~r-ni..ation ~vithout the use of ~ catalyst requires hi~her t.,.n~at-lres (110~l200~C) a~d a lon~er lenc,th of stay in the fumace. A simple pr~lon~ing of the le~xth of stay in the ~nace through enlargement ofthe furnace voIume, however has ~:he disadvanta~e o~lollger dead times. The same effect is stri.ven for in ~e kno~rn process in that thc sarnp~es ~aixed witb a carrier ~as are lead, on their way through the corn~ tion fi~m~ce, thro~gh t~e hottest furr~ce zones by means of nnetal sheets to change theLr d~rection ~disturbances), prior to Icaving the fumace, and are lcad to th~ ar~t messutement for ana~ysis.
The sample is placed into the furnace by mea~s of a lr~ns~l gas (c~rrier gas) and/o~
micro-nozzle dosing device. I~ doin~ so, the following contcxt is impo~tant:
The sarnple ~olume, ha~ng 2~100 micro 1iters, is ~ clr small It has to be injected i~to ~he combus~ion fLlmace alo~g ~~rith a carrier gas. llle carrier ga~ has ~e main function to transport ~e C~02-gas d~at has been obtained ~ough ~e combustion oue of the combustion fi~r~ace to an m~ared mea~ ment chamber. The an~o~mt of c~r~ie~ gas deterrnines the time period of the COZ exchasl~e in ~e combustion furnace. The amo~nt of thc carricr gas, h~wever, dilutes the product si~nal of t~e COZ to be measured ~rom whioh the TC, TOC etc are deteIminet.
In order to achieve a good entry of the effluent into the con~ Aon fumace given the aforementionet corlditions, a rne~nir.~l device has to t~yO~t ff~e samp~e with a high ~J~JI CU J~J ~LLJ I I ~)J 1111 L~ Il CA 022~33~4 199X-10-27 1 IJ~ ~U~ IV
.. . . . . .
ellergy ~ough a very ~hin noz~le into the combustion fiumace, or the liquid sa~ple has t~
be injected into the co~bustian furnace vvi~ the help of the c~r~e~ gas throug~L a lrex~r thi~l no~le (a nozzle with a v~ry s~nall cmss-section).
The ~ecess~ry obse~v~nce of t~e above~ "ltioned COII~itiOllS results in that the L~se of ti~e injection no~zles with a very sma~ tçr (5(~250 llm) very quicl~ly leads to the clo~ging up of the ~oz~te. If the nozle is enlarged, more calTier ~as has to be employed Ln orde~ to ~ozzle the mixnlre in the combustion film~ce with enouE~h enetg~r. In so doing, the product signal of the ~O~ is rcduced It is the~efore the object of t~e invention to arr~nge a process of the initially men~l~ned typc in such a w~y that, ill a s~mple vvay, a vely small ~ut very exactly determinable sample amount can be introduced intn the combus~ion fumace without that, in dou~g so, a ca~ier gas is u~ed a~d/or that the d~nger of the clogging of ~he thin lines e~ists l~e problem i~ solved according to the invention in that a liquid s~ ple h~n~ine onto a heating sur~ace is evapo~ated du~ing, a closed combustion fumace i~ order to ~ tS ;- \ the waste ~as sanlple to be lead to tl~e i~ d measu~ement, and ill that ~he pressure inc~ease in the combustion fu~nace ~enerated dur~ng the evapora~on or the humidity increase in the gas is meas~red ~nd, based on it, the sarnple an~ount is calculated.
In so doin~3, the separation of a ve~y small amount of sample occurs sunply for the reason that the ~mount of liquid that remains on ~he he~mg su~ace aI~ter the wctting of the heat~ surface with the li~uid ~onns the desired srna~l sample al lou~t, of wh~ch the voll~ne still has to be exac~ly doterrmned. This deternlination of Ihe vo1ume is conducted in a very sLmple n~ r~; ~rith high accuracy in that the ~l~iS~u~, increa~e that i~ cl ~Icd in the evaporntion or t~e humidity i~ c is measured. Tbis incr~ in the p~essure ~
case in the humidity can be lead m~ ically ba~ to thc e~ dted ~ou~t of the liquid.
In an especia~ly simple m~nn~r, ~e we~ting of the heat~Lg surface occurs in that th~
con~bustion furnace is at least partially filled with the Iiguid to bc ~ y~ed and iS then ~ . ~ . . . ~, .
~ U ~ h~J 11~ 1111 ~V~II CA 022~3354 1998-10-27 ~ UJU ~UCI I . ~
emp~ied throu~h the addition of gas The fnct that also the walls ~f ~e combustion furnace ~re ~ve~ed with the liquid does not mflllence the l,lea~u.~...en~ results bee~c the amount of the liquid h~neit~ on the ~alls is n~t ~.f..por~ted asld is thus nut considered i~
the analysi~.
~ device accordJn~ to the inve~tion for conducting the ~rocess that has a combustion furnace and a con~ectt~d device for infra~d meas.lr~lue,~lt is characterizcd in that the combus~o~ furnace h~s a fi~rnace C~A~ at can be closed, in which a h~ting eleme~t extends up~ard, and ~o ~hich a p~esslJre measuring device is at~ached.
Further adva~ta~geous embodiments of the spLnt of t}le invention are the obj~ct of fi~ er dependent claims.
In the ~ollowing, an example of an enlbotiment of the i~vention is de~c~ibet in det;ail as show~ in ~e diAgra~n.
The diagram shows, ih a ~imp~ified longitudi~al cr~o.s-~eclion, a device f~ the deterrnination of the C~llte"lt o~' o~idizable su~sl ~nees in aqueous liquids, especially the conte~t of carbon or nitrogen in e~ . ~ samp1e chamber I is a~ ,e~ in a me~uringb~oy 2 to be imm~ sed into the effluent to be analyzed. On the floor 3 of the chamber, a ch~mber open~ng S is arranged that can be closed usi~ a valve 4. Throu~h ~ ~s i~let valve 6 and a gas line 7 ~at extends upward fr~m the sample chamber 1, oxygen o~ (~o2_ free gas c~ be lead. As a 1pres~.ure l~leastllulg device, provided is a p~e~ mea~unng capsule 8 as ~ ed to the sample chamber 1. InYtead of this, also ~ humidity-measuring device can be provided. A gas-~elease valve Y serves to rele~se the g~ls fiom the ~.ample chamber 1. A~ a hes~ng element, a ~lowin~ wire 10 extends firom the sarnple chamber 1.
A dosing device 11 for the a~ldition of acid to chan~e the pH value is co~ected to the ssnlple chamber 1.
I~he sample chamber I which senre~ ~s reaction chaxnber or cornbustion filrnace is filled~
vl~en the valve 4 is opened and the gas-release valve 9 is open. with ~e cPfll~e~t ~o be ~ L~
~v ~ u ~ v ~1~1 .,., ~1, CA 0 2 2 5 3 3 5 4 19 9 8 - 10 - 2 7 ~ U ~, u . ~
.. . . . .................. _ . ..... . . ... ..
analyzed which flows through ~e charnber op~n-ng 5 illto the sample r~rnb~r 1 bymeans of the hydrostatic pressure of the ef~luent surroundin~ the n~ . ;n~ buoy 2. I hen the valve 4 is elosed. ~Jpon use of a p~-me~suring dcvice, a pH-value of, ~or example, 2-3 is set ~rou~h the addition of acid via a dosing device I I . The~ e s~nple ch~nber I is gassed via ~ gas-i~let ~ralve 6.
By mcans of the l~cnvt,~tu~g gas, dle ~1vater cQ~t~ined in the samplc chamber 1 is pushed out through the chamber opening 5 while the valve 4 is open. Then the val~e 4 on the charxlber floo~ 3 and the ~ in1et valve 6 are closed.
The he~ing element l O is we~ted ~vith a small anlount of the effluent to be analyzed. ~he heating element 10 is heated to l O00 120(~C for a short period of time. ~n so doing, the w~ter t~lat is adhering to the heatin~ element 10 is in.~t,..~ne~.usly evapotated arld increases the prcss~lre in the sample chamber l. l~merli~t~ly thereafter, the oxidizable substances contained in the w~te~ are burned to Co2 alld ~JO.
I~e pressure increase that is ge~erated by the e~a~ol~ali~ is ~neasured irl the pressure-measuring capsule 8 Instead o~this, al~o ~e h.~ ty inclcdse in the ga~ carl be mea~ured. From ~is~ the a~ ullt of the evaporated water is de~in~ n an ar~ly~er (not showxl he~e).
By opening the gas-inlet valve fi and the gas-release ~alve 9, the y,~ e~ l combus~on gas CO~ andJor NO are lead to a device (not shown here) fo~ the in~ared rneas~GI~c~t and a~e me~sured. rl~e value thus obtained equals, together w~th the amo~t of t~e evdpGr~d sample of wbich the volume has been determined from the pressure i~c.~eor fiom the hu~nidi~ increa~e, the content of oxidi~able substances, La the described example the content of c~rbon and/or nitrogen.
The ~rocess was described usin~ the e~mple of a n~e&~ing buoy immersed into thc ef~uent. ~t is ~mde~stood t}lat the process can also be adv~nta~eously enlployed in another ~5' ~JUI ~U UU ~ II'UU 1111 U~ I CA 02253354 1998-10-27 ' ~UJ U.1~J ~U~I ~, VU, IU
embodiment of the device, for exa~nple, when the ef~uent to be analyzed cont~ined in ~e sample ch~rnber is supplied via a line and a pump.
Claims (6)
C L A I M S
1. Process for the determination of the content of oxidzable substances in aqueous liquids, in which liquid samples are lead to a combustion furnace and are thermally treated, and the substance is burned to a gaseous oxide and, in a sample of the waste gas thus obtained, the content of the gaseous oxide is determined by means of infrared measurement, characterized in that a liquid sample hanging, onto a heating surface is evavorated during a closed combustion furnace in order to maintain the waste gas sample to be lead to the infrared measurement, and in that the pressure increase in the combustion furnace generated during the evaporation or the humidity increase in the gas is measured and, based on it, the sample amount is calculated.
2. Process according to claim 1, characterized in that the combustion furnace is at least partially filled with the liquid to be analyzed and is then emptied through the addition of gas.
3. Proccss according to claim 1, characterized in that the heating surface is heated to about 1000--1200°C.
4. Device for conducting the process according to one of claims 1 to 3, with a combustion furnace and a connected infrared measuring device, characterized in that the combustion furnace has a sample chamber (1) that can be closed, in which a heating element (10) extends upward, and to which a pressure-measuring device (8) is attached.
5. Device according to claim 4, characterised in that the heating element (10) has a glowing wire.
6. Device according to claim 4, characterized in that the sample chamber (1) is arranged in a measuring buoy to be immersed into the effluent to be analyzed and that on the floor (3) of the chamber, a chamber opening (5) is arranged that can be closed using a valve (4).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19617910A DE19617910B4 (en) | 1996-05-03 | 1996-05-03 | Method and device for determining the content of oxidisable ingredients in aqueous liquids |
| DE19617910.6 | 1996-05-03 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2253354A1 true CA2253354A1 (en) | 1997-11-13 |
Family
ID=7793319
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002253354A Abandoned CA2253354A1 (en) | 1996-05-03 | 1997-04-26 | Process and device for determining the oxidisable substance content of aqueous liquids |
Country Status (8)
| Country | Link |
|---|---|
| EP (1) | EP0896670B1 (en) |
| JP (1) | JP3626205B2 (en) |
| AT (1) | ATE269540T1 (en) |
| CA (1) | CA2253354A1 (en) |
| DE (2) | DE19617910B4 (en) |
| DK (1) | DK0896670T3 (en) |
| ES (1) | ES2224243T3 (en) |
| WO (1) | WO1997042499A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009001860A1 (en) | 2009-03-25 | 2010-09-30 | Endress + Hauser Conducta Gesellschaft für Mess- und Regeltechnik mbH + Co. KG | Method for determining a number of drops |
| DE102009001861A1 (en) | 2009-03-25 | 2010-09-30 | Endress + Hauser Conducta Gesellschaft für Mess- und Regeltechnik mbH + Co. KG | Method for operating an analysis device |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3567387A (en) * | 1969-01-09 | 1971-03-02 | Westinghouse Electric Corp | Carbon dioxide monitor |
| US3892528A (en) * | 1973-04-02 | 1975-07-01 | Oceanography Int Corp | Method and apparatus for vaporizing liquids to be contacted with a carrier gas |
| US4089209A (en) * | 1977-08-04 | 1978-05-16 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Remote water monitoring system |
| DE2811135C2 (en) * | 1978-03-15 | 1986-04-24 | Hoechst Ag, 6230 Frankfurt | Method for the quantitative determination of carbon organic compounds in water |
| DE3935720A1 (en) * | 1989-10-27 | 1991-05-02 | Krc Umwelttechnik Gmbh | METHOD FOR DETERMINING THE CARBONATE CONTENT OF WASHING SUSPENSIONS |
| DE4344441C1 (en) * | 1993-12-24 | 1995-07-13 | Siepmann Friedrich W | Method and device for the continuous determination of the content of oxidizable ingredients in aqueous liquids |
-
1996
- 1996-05-03 DE DE19617910A patent/DE19617910B4/en not_active Expired - Fee Related
-
1997
- 1997-04-26 ES ES97921792T patent/ES2224243T3/en not_active Expired - Lifetime
- 1997-04-26 CA CA002253354A patent/CA2253354A1/en not_active Abandoned
- 1997-04-26 DE DE59711724T patent/DE59711724D1/en not_active Expired - Lifetime
- 1997-04-26 JP JP53949097A patent/JP3626205B2/en not_active Expired - Fee Related
- 1997-04-26 EP EP97921792A patent/EP0896670B1/en not_active Expired - Lifetime
- 1997-04-26 WO PCT/EP1997/002165 patent/WO1997042499A1/en active IP Right Grant
- 1997-04-26 AT AT97921792T patent/ATE269540T1/en not_active IP Right Cessation
- 1997-04-26 DK DK97921792T patent/DK0896670T3/en active
Also Published As
| Publication number | Publication date |
|---|---|
| EP0896670A1 (en) | 1999-02-17 |
| EP0896670B1 (en) | 2004-06-16 |
| JP2001503850A (en) | 2001-03-21 |
| ES2224243T3 (en) | 2005-03-01 |
| ATE269540T1 (en) | 2004-07-15 |
| DE19617910B4 (en) | 2007-03-01 |
| JP3626205B2 (en) | 2005-03-02 |
| WO1997042499A1 (en) | 1997-11-13 |
| DE19617910A1 (en) | 1997-11-13 |
| DE59711724D1 (en) | 2004-07-22 |
| DK0896670T3 (en) | 2004-10-18 |
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| FZDE | Discontinued |