GB1591368A - Apparatus for analysis of samples by combustion - Google Patents
Apparatus for analysis of samples by combustion Download PDFInfo
- Publication number
- GB1591368A GB1591368A GB3554776A GB3554776A GB1591368A GB 1591368 A GB1591368 A GB 1591368A GB 3554776 A GB3554776 A GB 3554776A GB 3554776 A GB3554776 A GB 3554776A GB 1591368 A GB1591368 A GB 1591368A
- Authority
- GB
- United Kingdom
- Prior art keywords
- gas
- combustion
- sample
- nitrogen
- loop
- 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
Links
- 238000002485 combustion reaction Methods 0.000 title claims description 37
- 238000004458 analytical method Methods 0.000 title claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 54
- 239000007789 gas Substances 0.000 claims description 37
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 17
- 239000001569 carbon dioxide Substances 0.000 claims description 17
- 238000005070 sampling Methods 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229910001868 water Inorganic materials 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 239000000567 combustion gas Substances 0.000 claims description 11
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 claims description 4
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002250 absorbent Substances 0.000 claims description 2
- 230000002745 absorbent Effects 0.000 claims description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims description 2
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 claims description 2
- 239000003085 diluting agent Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 2
- 229960003540 oxyquinoline Drugs 0.000 claims description 2
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229960004643 cupric oxide Drugs 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 239000008262 pumice Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 239000003701 inert diluent Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (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)
Description
(54) APPARATUS FOR ANALYSIS OF SAMPLES BY. COMBUSTION
(71) We, THE INTERNATIONAL SYN- THETIC RUBBER COMPANY LIMITED, a British
Company, of Brunswick House, Brunswick
Place, Southampton, Hampshire, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: This invention relates to an apparatus for use in the analysis of samples by combustion. In a particular embodiment it relates to an apparatus for the combustion of a solid or liquid material in the determination of its nitrogen, carbon or hydrogen content.
It is well known to determine the nitrogen, carbon or hydrogen content of a solid or liquid material by combustion of a weighed sample of the material in a combustion zone in a stream of oxygen and to determine the nitrogen, carbon or hydrogen content, as the case may be, of the combustion gas. In this specification the expression "combustion gas" is used to indicate the gas resulting from combustion of the sample. The combustion gas will, of course, comprise both the products of combustion and oxygen. One problem which occurs in such a method is the incomplete combustion of the sample leading to a result which is lower than the true figure. Further, in known apparatus a gas other than oxygen is used to flush the combustion gas from the combustion zone.
We have now found that these disadvantages may be obviated Iby recycling the combustion gas several times through the combustion zone using a closed loop system.
According to the present invention an apparatus for use in the analysis of a sample by combustion comprises a combustion'zone having an inlet and an outlet, a tubular loop linking the inlet to the outlet, a constant volume pump in the loop, a sample port for introducing the sample to be analysed into the combustion zone, a gas inlet to the loop ahead of the combustion zone and a gas sampling valve for extracting a measured volume of the gas circulated in the loop by the constant volume pump when the apparatus is in use.
One embodiment of the invention will now be described with reference to the drawing, filed with the Provisional Specification, which is a schematic diagram of the apparatus of this embodiment.
In this embodiment the apparatus comprises a combustion tube 1, a sample port 2, a gas inlet 3, a constant volume pump 4, and a gas sampling valve 5. In the case of nitrogen analysis, a carbon dioxide absorption tube 6, may be inserted in the loop or fitted to the outlet side of the gas sampling valve. However, the use of this tube is op tonal. The combustion tube 1, may be, for example, a straight tube approximately 60 cms. long of 2 to 2.5 cms. bore and may be made of fused quartz. The volume of the tube governs the volume of the apparatus and thus the size of sample required for a given sensitivity. The tube is loosely packed with a catalyst the function af which is to ensure combustion of the sample and conversion of the combustion product into nitrogen, carbon dioxide and/or water vapour.A suitable material is, for example, cupric oxide deposited on alumina or silica gel. Other oxygen donors may, of course, be used. If desired a layer of platinised pumice may be deposited on top of the catalyst to ensure immediate ignition. A cylinder of copper gauze may be inserted above the catalyst, ensuring good contact with the wall of the combustion tube so that in use the gauze oxidises to copper oxide assisting combus tibn of the vaporised sample. The constant volume pump is conveniently of the peri static type, a typical model b'eing the HR
Flow Inducer Type MHRK, made by The
Watson Mallow Air Pump Co. Desirably the loop, the sampling valve and the combustion tube are temperature controlled.This is especially important where the hydrogen content of a sample is to be determined since the system must be, maintained above the dew point of the circulating gases. If used in nitrogen analysis, the absorption tube, 6, removes carbon dioxide, hydrogen, sulphur oxides and possibly halogens. It may ibe packed with soda-asbestos mixed with pumice or other inert diluent. The diluent prevents clogging and ensures free passage of combustion gas through the absorption tube.
The gas sampling valve 5, is used to extract a measured volume of gas and to inject this into a detector/analyser for determination of the desired content. A volume of 1 to 2 -cc. is normally adequate. A suit able-valve is that manufactured by Perkin
Elmer for their gas chromatographs. The gas inlet 3, may be a simple diaphragm or similar valve and is used to supply oxygen at a fixed over-pressure to the loop. It is conveniently set at -t- or 1 psig.
In use the apparatus of the invention is connected to a, suitable detector/analyser.
One form of detector/analyser comprises a separating column packed with molecular sieve Grade 5A or 13 X and a katharometer detector. Alternatively a commercial gas liquid chromatograph (GLC) equipped with a helium carrier-gas line may be used. A suitable chromatograph is the Perkin Elmer
Model 452.
To operate the apparatus of the invention the combustion tube 1, is heated to a suitable temperature, for example, 500"C to 1,000 C and oxygen is supplied to the apparatus through the gas inlet 3, at a pressure of, for example, 21 pslig. The gas sampling valve 5, lis closed and the constant volume pump 4, is started to circulate the oxygen. A weighed sample of the material to be analysed, weighing, for example, 10 to 40 mug., is introduced into the combustion tube 1, via sample port 2, which is promptly closed. Combustion of the sample occurs and the combustion gas is circulated around the loop.After a short interval, for example, 5 minutes to enable the system to equilibriate, a known volume sample of the circulating gas is extracted and passed to the detector/analyser for determination of the nitrogen, carbon or hydrogen content as the case may be. The apparatus is flushed with oxygen vented through sample port 2, and is ready for further use.
When nitrogen or carbon dioxide or water is released from the sample its partial pressure is determined by the quantity and the volume and temperature(s) of the loop. It is iindependent of the total gas pressure. The gas sampling valve supplies a measured volume of the atmosphere within the loop to an' analyser which measures the quantity of nitrogen or carbon or water in the sample.
The apparatus may be standardised using samples of known nitrogen, carbon or hydrogen content, for example, 8-hydroxyquinoline so that the detector/analyser may be
calibrated and a direct reading of the re
quired content obtained.
The apparatus of the invention is especially
useful for the determination of the nitrogen content-of a wide variety of'samples and pro
vides a cheap, speedy and reliable method for doing so. It is particularly applicable to
the determination of the acrylonitr'ile'còn- tent of acrylonitrile butadiene styrene (ABS) plastics.
In the determination of all'three elements, carbon, hydrogen and nitrogen, the apparatus can be operated on the su;btractive principle. Carbon dioXide absorption tube 6, is omitted but may be replaced by a heated
tube to remove the sulphur oxides and halogens, packed with absorbents such as lead
chromate or silver. Oxygen is first removed by reaction with hot copper. The combustion gas containing carbon dioxide, water and nitrogen is passed in succession through first a katharometer cell, a water absorber such as anhydrone, a second katharometer, a carbon dioxide absorber such as sodaasbestos/anhydrone and finally a third katharometer. By matching the response factors of the detectors the amounts of carbon dioxide, hydrogen and nitrogen can readily be derived.Alternatively two sampling valves may be used to transmit samples to two columns in parallel. Carbon dioxide and water are removed from one sample and this is passed to a column which separates oxygen and nitrogen so that these will occur as two separate peaks. A second column separates oxygen/nitrogen, carbon dioxide and water so that these may be detected as separate peaks. Other ways of linking the apparatus of the invention to the detector/analyser may be envisaged such as the use of a second gas sampling valve linked to that employed in the apparatus to enable hydrogen carrier-gas to be used safely for the GLC analysis.
WHAT WE CLAIM IS: 1. Apparatus for use in the analysis of a sample by combustion comprising a combustion zone having an inlet and an outlet, a tubular loop linking the inlet to the outlet, a constant volume pump in the loop, a sample port for introducing the sample to be analysed into the combustion zone, a gas inlet to the loop ahead of the combustion zone and a gas sampling valve for extracting a measured volume of the gas circulated in the loop by the constant volume pump when the apparatus is in use.
2. Apparatus for use in the analysis for nitrogen content of a sample by combustion substantially as hereinbefore described with
**WARNING** end of DESC field may overlap start of CLMS **.
Claims (4)
1. Apparatus for use in the analysis of a sample by combustion comprising a combustion zone having an inlet and an outlet, a tubular loop linking the inlet to the outlet, a constant volume pump in the loop, a sample port for introducing the sample to be analysed into the combustion zone, a gas inlet to the loop ahead of the combustion zone and a gas sampling valve for extracting a measured volume of the gas circulated in the loop by the constant volume pump when the apparatus is in use.
2. Apparatus for use in the analysis for nitrogen content of a sample by combustion substantially as hereinbefore described with
reference to and as shown in the drawing accompanying the Provisional Specification.
3. A method of analysis employing the apparatus of claim 1 or claim 2 substantially as hereinbefore described.
4. A method of analysis substantially as hereiitbefore described with reference to the Drawing accompanying the Provisional
Specification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB3554776A GB1591368A (en) | 1977-11-28 | 1977-11-28 | Apparatus for analysis of samples by combustion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB3554776A GB1591368A (en) | 1977-11-28 | 1977-11-28 | Apparatus for analysis of samples by combustion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1591368A true GB1591368A (en) | 1981-06-17 |
Family
ID=10378947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB3554776A Expired GB1591368A (en) | 1977-11-28 | 1977-11-28 | Apparatus for analysis of samples by combustion |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB1591368A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0964248A1 (en) * | 1998-06-12 | 1999-12-15 | Horiba, Ltd. | System for analyzing elements in sample |
| GB2446824A (en) * | 2007-02-26 | 2008-08-27 | Thermo Fisher Scientific Inc | Apparatus and method for detecting incomplete combustion in a combustion analyser |
| CN109459525A (en) * | 2018-12-27 | 2019-03-12 | 山东宏业纺织股份有限公司 | A kind of device and test method improving flame-retardant yarn flame retardant property testing precision |
| CN114965834A (en) * | 2022-06-10 | 2022-08-30 | 长沙开元弘盛科技有限公司 | A method and device for determining nitrogen content in non-gaseous samples |
-
1977
- 1977-11-28 GB GB3554776A patent/GB1591368A/en not_active Expired
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0964248A1 (en) * | 1998-06-12 | 1999-12-15 | Horiba, Ltd. | System for analyzing elements in sample |
| US6627155B1 (en) | 1998-06-12 | 2003-09-30 | Horiba, Ltd. | Combustion furnace system for analyzing elements in a sample |
| GB2446824A (en) * | 2007-02-26 | 2008-08-27 | Thermo Fisher Scientific Inc | Apparatus and method for detecting incomplete combustion in a combustion analyser |
| GB2446824B (en) * | 2007-02-26 | 2009-06-17 | Thermo Fisher Scientific Inc | Apparatus and method for detecting incomplete combustion in a combustion analyser |
| CN109459525A (en) * | 2018-12-27 | 2019-03-12 | 山东宏业纺织股份有限公司 | A kind of device and test method improving flame-retardant yarn flame retardant property testing precision |
| CN109459525B (en) * | 2018-12-27 | 2024-01-19 | 山东宏业纺织股份有限公司 | Device for improving flame retardant property test accuracy of flame retardant yarns |
| CN114965834A (en) * | 2022-06-10 | 2022-08-30 | 长沙开元弘盛科技有限公司 | A method and device for determining nitrogen content in non-gaseous samples |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed | ||
| PCNP | Patent ceased through non-payment of renewal fee |