CN202661431U - Measuring instrument for particulate organic carbon and total organic carbon - Google Patents

Measuring instrument for particulate organic carbon and total organic carbon Download PDF

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Publication number
CN202661431U
CN202661431U CN 201220342506 CN201220342506U CN202661431U CN 202661431 U CN202661431 U CN 202661431U CN 201220342506 CN201220342506 CN 201220342506 CN 201220342506 U CN201220342506 U CN 201220342506U CN 202661431 U CN202661431 U CN 202661431U
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organic carbon
quartz
quartz ampoule
communicated
reactor
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徐惠忠
徐滋秋
毕国明
张俊华
徐成彬
陈静
李云东
李圣伟
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Yantai University
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Yantai University
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Abstract

The utility model relates to a measuring instrument for particulate organic carbon and total organic carbon. The measuring instrument is characterized in that a carrier gas generator is communicated with a gas purifying device and a flow rate controller sequentially through pipelines, wherein the flow rate controller is respectively communicated with a high-temperature oxidation reactor and a low-temperature decomposing reactor through pipelines; the other ends of the high-temperature oxidation reactor and the low-temperature decomposing reactor are respectively communicated with a condensing dewatering device; the condensing dewatering device, an ion trap, a gas filtering device and an electric conductivity meter are sequentially communicated through the pipelines; and the electric conductivity meter and a data processor are connected via a cable. With the adoption of the measuring instrument for particulate organic carbon and total organic carbon provided by the utility model, the total carbon, the inorganic carbon, the particulate organic carbon, the total organic carbon and the like in a solid sample, a particle sample, a liquid sample and a suspension sample can be measured, thus, the particulate organic carbon in the soil, sludge, organic chemical residue and the like, and the total organic carbon in surface water, domestic sewage and production wastewater can be measured; the measuring instrument has a wide measurement scope, is convenient to use, has the capacity of carrying out laboratory measuring and vehicle-mounted flowing detecting, and is worthy of being popularized.

Description

A kind of particulate organic carbon, total organic carbon analyzer
Technical field
The utility model relates to the organic carbon determination instrument in a kind of solid, liquid, the granular substance, relates in particular to a kind of particulate organic carbon, total organic carbon analyzer.
Background technology
Organic of a great variety, quantity is large, it is wide to distribute, no matter be in the sky or on the ground, underground, be the trace that residue that air or surface water, sanitary sewage, factory effluent, soil, bed mud, organic chemical industry produce all has them.Organic assay method has biochemical oxygen demand (BOD), chemical oxygen demand (COD) (COD), total oxygen utilization (TOD), ultraviolet absorptivity (UV ASM) and total organic carbon (TOC).Biochemical oxygen demand, total oxygen utilization and ultraviolet absorptivity method can only be measured the organic content in the water, though COD Determination Method can be measured the organism in solid, the granule, operation steps is various, minute is long, can not realize automatic mensuration, can not instrumentation.Only have the determining total organic carbon method can measure particulate organic carbon (Particulate Organic Carbon is called for short POC) and SOLID ORGANIC carbon (Solid Organic Carbon is called for short SOC).
Still do not have at present special-purpose POC analyzer both at home and abroad, only have extremely indivedual model total organic carbon (Total Organic Carben is called for short TOC) analyzers of extremely indivedual foreign manufacturers can finish the mensuration of part particulate organic carbon.The deficiency that exists mainly contains: can not measure the high particle of salt content, such as salt water lake and ocean bed mud, such as the residue that produces in the industry production processes such as agricultural chemicals and chemical fertilizer, dyestuff, seaization, salinization; Service condition is harsh, use high-purity steel cylinder gas, is difficult to vehicle-mounted floating mensuration, on-site measurement; Testing sample in advance acidifying is removed inorganic carbon, then oven dry, the sample that quantitatively takes by weighing again after the baking is put platinum boat or the quartz boat that band transmits bar into, above operation steps can make the carbon dioxide in the dry sample absorbed air of having removed inorganic carbon, load weighted sample has loss when pouring platinum boat or quartz boat into, causes the larger data error; Platinum boat or quartz boat are when delivering to 980 ℃ of high-temperature regions with sample, because connecting rod push-and-pull campaign, the sealing gasket of wearing and tearing can be oxidized to carbon dioxide and gas leakage, affects the precision of instrument; Infrared detector is expensive, the instrument price is high, is difficult to promote.
Summary of the invention
The purpose of this utility model provide a kind of simple in structure, dependable performance, cost low, disturb few particulate organic carbon, total organic carbon analyzer.
The technical solution of the utility model is:
A kind of particulate organic carbon, total organic carbon analyzer, characteristics are, pass through successively pipeline communication between carrier gas generator and gas purifier, the flow controller, flow controller is communicated with respectively high-temperature oxydation reactor and low-temperature decomposition reactor by pipeline, the other end of high-temperature oxydation reactor and low-temperature decomposition reactor is communicated with the condensation hydroextractor respectively by pipeline, successively by pipeline communication, be connected by cable between conductivity meter and the data processor between condensation hydroextractor, ion trap, gas filter, the conductivity meter.
Described high-temperature oxydation reactor includes the high-temperature oxydation reactor base, be provided with the quartz ampoule support in the high-temperature oxydation reactor base, the quartz ampoule support is provided with quartz ampoule, end at quartz ampoule is provided with the sample feeding pipe mouth of pipe, in quartz ampoule, be movably equipped with the sample converyer corresponding to the sample feeding pipe mouth of pipe, outside at the quartz ampoule other end is provided with pyrostal, the two ends of quartz ampoule are respectively equipped with carrier gas draft tube and reaction gas escape pipe, the carrier gas draft tube is communicated with flow controller, and the reaction gas escape pipe is communicated with the condensation hydroextractor.
Described low-temperature decomposition structure of reactor and high-temperature oxydation reactor are roughly the same, and difference is that what to arrange in the outside of the quartz ampoule other end is cryostat.
The described sample converyer structure that is arranged in high-temperature oxydation reactor or the low-temperature decomposition reactor is the same, it includes quartz ring, be connected with the quartz ring connecting rod at quartz ring, the quartz ring connecting rod is provided with the magnetic post, be provided with the magnet ring track at the quartz ampoule support, be movably equipped with magnet ring on the magnet ring track, magnet ring is corresponding with the magnetic post, be movably equipped with quartz curette at quartz ring, quartz curette is corresponding with the sample feeding pipe mouth of pipe of quartz ampoule.
Described conductivity meter comprises conductance cell, conductance cell is communicated with respectively base exchanger, gas purifier by pipeline, one end of conductance cell is communicated with gas filter by pipeline, and the conductance electrode of conductance cell connects electricity by cable and leads controller, and electricity is led controller and is connected with data processor.In above-mentioned, can also be equipped with electricity between conductance cell and gas purifier again and lead reactor, base exchanger also can change base reagent into.
Compared with the prior art, analyzer of the present utility model has interference and lacks, dependable performance, low cost and other advantages, utilize the utility model can measure respectively solid sample, particulate samples, liquid, total carbon in the suspended matter sample, inorganic carbon, particulate organic carbon, total organic carbon etc., thereby realization soil, mud, particulate organic carbon and the surface water such as organic chemical industry's residue, sanitary sewage, the mensuration of total organic carbon in the factory effluent, measurement range is wide, because it is simple in structure, easy to use, both can carry out measuring in the good environment in laboratory, also can not carry danger, heavy steel cylinder carries out flow assay at monitoring car, is worthy to be popularized very much.
For clearly demonstrating the technical solution of the utility model, do simple the introduction below in conjunction with drawings and Examples.
Description of drawings
Fig. 1 is the disclosed a kind of structural representation of the utility model embodiment;
Fig. 2 is the disclosed another kind of structural representation of the utility model embodiment;
Fig. 3 is the structural representation of the disclosed high-temperature oxydation reactor of the utility model embodiment;
Fig. 4 is the structural representation of the disclosed low-temperature decomposition reactor of the utility model embodiment.
The explanation of accompanying drawing drawing:
1 carrier gas generator, 3 high-temperature oxydation reactors, 4 low-temperature decomposition reactors, 5 condensation hydroextractors, 6 ion traps, 7 gas filters, 8 conductivity meters, 9 data processors,
17 gas purifiers, 18 flow controllers, 19 flow controllers,
21 T-valve, 22 T-valve, 23 T-valve, 24 T-valve, 25 T-valve,
30 catalyzer, 31 quartz ampoules, the 311 sample feeding pipe mouths of pipe, 312 quartz ampoule pipe mouth sealing plugs, 313 quartz ampoule supports, 32 carrier gas draft tube, 33 reaction gas escape pipes, 34 quartz curettes, 35 quartz rings, 351 quartz ring connecting rods, 36 magnetic posts, 37 magnet rings, 371 magnet ring tracks, 38 high-temperature oxydation reactor base, 381 insulation claddings, 382 pyrostals
40 acidulants, 41 quartz ampoules, the 411 sample feeding pipe mouths of pipe, 412 quartz ampoule pipe mouth sealing plugs, 413 quartz ampoule supports, 42 carrier gas draft tube, 43 reaction gas escape pipes, 44 quartz curettes, 45 quartz rings, 451 quartz ring connecting rods, 46 magnetic posts, 47 magnet rings, 471 magnet ring tracks, 48 low-temperature decomposition reactor base, 481 insulation claddings, 482 cryostats
80 electricity are led controller, 81 conductance cells, and 811 conductance electrodes, 82 base exchangers, 83 electricity are led reactor, 84 peristaltic pumps, 85 base reagents, 88 power supplys,
91 displays and printer, 92 data transmission terminals, 93 keyboards.
Embodiment
Fig. 1 is the disclosed a kind of particulate organic carbon of the utility model embodiment, total organic carbon analyzer structural drawing, and wherein 1 is that carrier gas generator, 17 is that gas purifier, 18,19 is that flow controller, 21,22,23,24,25 is that T-valve, 3 is that high-temperature oxydation reactor, 4 is that low-temperature decomposition reactor, 5 is that condensation hydroextractor, 6 is that ion trap, 7 is that gas filter, 8 is that conductivity meter, 9 is data processor; Carrier gas generator 1 and gas purifier 17, flow controller 18, pass through pipeline communication between the T-valve 21, T-valve 21 and high-temperature oxydation reactor 3, pass through pipeline communication between the T-valve 22, T-valve 21 and low-temperature decomposition reactor 4, pass through pipeline communication between the T-valve 22, T-valve 22 and condensation hydroextractor 5, ion trap 6, gas filter 7, T-valve 23, pass through successively pipeline communication between the conductivity meter 8, wherein in the conductivity meter 8, pass through pipeline communication between T-valve 23 and the conductance cell 81, T-valve 23, T-valve 24, pass through pipeline communication between the base exchanger 82, base exchanger 82 and peristaltic pump 84, pass through pipeline communication between the T-valve 24, conductance cell 81 and T-valve 25, gas purifier 17, pass through pipeline communication between the flow controller 19, conductance cell conductance electrode 811 is led controller 80 with electricity, connect by cable between the data processor 9, electricity is led controller 80, data processor 9 connects respectively power supply 88, can connect display and printer 91 on the data processor 9, data transmission terminal 92, the auxiliary equipment such as keyboard 93.
Fig. 2 is the disclosed another kind of particulate organic carbon of the utility model embodiment, total organic carbon analyzer device structural drawing, the disclosed structure of its structure and Fig. 1 is roughly the same, difference is, structure in the conductivity meter 8 is different, referring to Fig. 2, T-valve 23, pass through pipeline communication between T-valve 24 and the conductance cell 81, conductance cell 81, T-valve 24, peristaltic pump 84, pass through pipeline communication between the base reagent 85, T-valve 23, electricity is led reactor 83, T-valve 25, gas purifier 17, by pipeline communication, conductance cell conductance electrode 811 is led controller 80 with electricity between the flow controller 19, connect by cable between the data processor 9.
Fig. 3 is high-temperature oxydation structure of reactor figure, include high-temperature oxydation reactor base 38, be provided with quartz ampoule support 313 in high-temperature oxydation reactor base 38, quartz ampoule support 313 is provided with quartz ampoule 31, end at quartz ampoule 31 is provided with the sample feeding pipe mouth of pipe 311, in quartz ampoule 31, be movably equipped with the sample converyer corresponding to the sample feeding pipe mouth of pipe 311, be provided with the high-temperature oxydation district at quartz ampoule 31 other ends, there is catalyzer 30 the inside in high-temperature oxydation district, the outside in high-temperature oxydation district is provided with 980 ℃ of pyrostals 382, insulation cladding 381 is arranged outside the pyrostal 382, the two ends of quartz ampoule 31 are respectively equipped with carrier gas draft tube 32 and reaction gas escape pipe 33, wherein, carrier gas draft tube 32 and T-valve 21, flow controller 18 is communicated with, reaction gas escape pipe 33 and T-valve 22, condensation hydroextractor 5 is communicated with, and goes out to be provided with the quartz ampoule pipe mouth sealing plug at the quartzy mouth of pipe.
Above-mentioned sample converyer includes quartz ring 35, be connected with quartz ring connecting rod 351 at quartz ring 35, quartz ring connecting rod 351 is provided with magnetic post 36, be provided with magnet ring track 371 at quartz ampoule support 313, be movably equipped with magnet ring 37 on the magnet ring track 371, magnet ring 37 positions are corresponding with magnetic post 36, and activity is placed with quartz curette 34 on quartz ring 35, and the position of quartz curette 34 is corresponding with the sample feeding pipe mouth of pipe 311 above the quartz ampoule 31.
Fig. 4 is low-temperature decomposition structure of reactor figure, the low-temperature decomposition reactor is substantially the same with the structure of high-temperature oxydation reactor, difference is to be provided with the low-temperature decomposition district at the quartz ampoule other end, there is acidulant 40 the inside in low-temperature decomposition district, the outside in low-temperature decomposition district is provided with 150 ℃ of cryostats 482, other structures are with just the same with the high-temperature oxydation reactor, and relevant label declaration is referring to the explanation of accompanying drawing drawing, and structure repeats no more.
The below utilizes the utility model analyzer to carry out the assay method of particulate organic carbon, total organic carbon with the experimental example summary.
One, particulate organic carbon is measured ultimate principle and step:
1, testing sample pre-service: solid and grind greater than 30 purpose particulate samples and to sieve, in 115 ℃ baking oven, toast 2h, put into again exsiccator and cool off;
2, testing sample collection: with the cleaned quartz curette of washing lotion, take by weighing quantitative testing sample (0.3 ~ 1g);
3, sample is put into the high-temperature oxydation reactor: the quartz curette that testing sample is housed is put into quartz ring, screw the sample feeding pipe mouth of pipe and sealing;
4, sample is brought the high-temperature oxydation district into: slip magnet ring band is automatically connected in the quartz ring on the magnetic post, quartz curette is sent to 980 ℃ high-temperature oxydation district, makes all kinds of organic carbons and inorganic carbon in the sample all be converted into carbon dioxide:
Figure 314511DEST_PATH_IMAGE001
5, the mensuration of carbon dioxide: entered in the conductivity meter with the carbon dioxide that oxidation in the above-mentioned steps produces by carbon-free carrier gas, with the alkaline electro drain generation neutralization reaction in the conductivity meter, namely:
Figure 293968DEST_PATH_IMAGE002
Because OH -With CO 3 2-Variation be directly proportional with the quantity of carbon dioxide, the variation of conductivity is the total carbon of testing sample;
6, the data of total carbon content are processed: the signal that conductivity meter detects is sent to data processor by cable, is calculated, stored, shows, prints again total carbon (TC) content of particulate organic matter by the software that pre-deposits and calibration curve;
7, sample is put into the low-temperature decomposition reactor: putting into quartz ring with the quartz curette that testing sample is housed of (2) step equivalent, add the phosphoric acid of 0.1 ~ 0.5mL in the quartz curette, screw the sample feeding pipe mouth of pipe and sealing;
8, sample is put into the low-temperature decomposition district: slip magnet ring band is automatically connected in and gets quartz ring on the magnetic post, quartz curette is sent to 150 ℃ low-temperature decomposition district, and all kinds of inorganic carbons in the sample are converted into carbon dioxide:
Figure 634557DEST_PATH_IMAGE003
9, the mensuration of carbon dioxide: carbon-free carrier gas enters in the conductivity meter with decomposing the carbon dioxide that produces in the above-mentioned steps, with the alkaline electro drain generation neutralization reaction in the conductivity meter, with (5) step, conductivity is changed:
Figure 92083DEST_PATH_IMAGE004
10, the data of inorganic carbon content are processed: the detection signal of conductivity meter is sent to data processor by cable, goes out particulate inorganic carbon (IC) content by the software that pre-deposits and standard correction curve calculation, storage, Display and Print;
11, by data processor calculating, storage, Display and Print particulate organic carbon (POC) content:
TC–IC = POC 。
Two, determining total organic carbon principle and step :
Total organic carbon is the overall target that represents Organic Pollution in the water with the content of carbon, can more directly reflect the self-purification capacity of water body organic compound.Total organic carbon has dry oxidation determination method and wet oxidation determination method.General dry method instrument palpus filtering can cause the loss of organic carbon greater than the particle of 100um, the impurity that an assay method of the present invention and instrument filtering 500um is above, and the loss that causes is few.
1, testing sample pre-service: sample refrigerates otherwise will add mercuric sulfate with to survey, processes or shakes up with the ultrasonic transmitter homogenizing before measuring;
2, testing sample collection: draw 0.05 ~ 1mL water sample to be measured with self-priming automatic sampler;
3, sample is put into the high-temperature oxydation reactor: water sample is injected quartz curette, screw the sample feeding pipe mouth of pipe and sealing;
4, sample is brought the high-temperature oxydation district into: identical with particulate organic carbon determination step 4;
5, the mensuration of carbon dioxide: identical with particulate organic carbon determination step 5;
6, the data of total carbon content are processed: identical with particulate organic carbon determination step 6;
7, sample is put into the low-temperature decomposition reactor: the water sample with (2) step equivalent is injected quartz curette, screw the sample feeding pipe mouth of pipe and sealing;
8, sample is sent into the low-temperature decomposition district: identical with particulate organic carbon determination step 8;
9, the mensuration of carbon dioxide: identical with particulate organic carbon determination step 9;
10, the data of inorganic carbon content are processed: identical with particulate organic carbon determination step 10;
11, by data processor calculating, storage, Display and Print total organic carbon (TOC) content:
TC–IC = TOC 。
In addition, nitrogen phosphate and sulfur in the sample and halogen compound can be converted into corresponding oxide under the effect of 980 ℃, catalyzer and oxygen, these oxides enter electricity and lead detector and will produce the output of corresponding signal under the drive of carrier gas, interference detector is to the mensuration of carbon dioxide, even pollution detection instrument and the pipeline that links to each other.To this, can in ion trap 6 of the present utility model, arrange and comprise silver manganate porous particle, silver oxide porous particle, oxidation filamentary silver conveyor screw, filamentary silver conveyor screw, cathode copper particle etc., activity and the specific surface area of these materials are large, can rapid reaction eliminate its interference.

Claims (7)

1. particulate organic carbon, total organic carbon analyzer, it is characterized in that, carrier gas generator (1) and gas purifier (17), flow controller passes through pipeline communication between (18) successively, flow controller (18) is communicated with respectively high-temperature oxydation reactor (3) and low-temperature decomposition reactor (4) by pipeline, the other end of high-temperature oxydation reactor (3) and low-temperature decomposition reactor (4) is communicated with condensation hydroextractor (5) respectively by pipeline, condensation hydroextractor (5), ion trap (6), gas filter (7), successively by pipeline communication, be connected by cable between conductivity meter (8) and the data processor (9) between the conductivity meter (8).
2. a kind of particulate organic carbon according to claim 1, total organic carbon analyzer, it is characterized in that, described high-temperature oxydation reactor (3) includes high-temperature oxydation reactor base (38), be provided with quartz ampoule support (313) in high-temperature oxydation reactor base (38), quartz ampoule support (313) is provided with quartz ampoule (31), end at quartz ampoule (31) is provided with the sample feeding pipe mouth of pipe (311), in quartz ampoule (31), be movably equipped with the sample converyer corresponding to the sample feeding pipe mouth of pipe (311), outside at quartz ampoule (31) other end is provided with pyrostal (382), the two ends of quartz ampoule (31) are respectively equipped with carrier gas draft tube (32) and reaction gas escape pipe (33), carrier gas draft tube (32) is communicated with flow controller (18), and reaction gas escape pipe (33) is communicated with condensation hydroextractor (5).
3. a kind of particulate organic carbon according to claim 2, total organic carbon analyzer, it is characterized in that, described sample converyer includes quartz ring (35), be connected with quartz ring connecting rod (351) at quartz ring (35), quartz ring connecting rod (351) is provided with magnetic post (36), be provided with magnet ring track (371) at quartz ampoule support (313), be movably equipped with magnet ring (37) on the magnet ring track (371), magnet ring (37) is corresponding with magnetic post (36), be movably equipped with quartz curette (34) at quartz ring (35), quartz curette (34) is corresponding with the sample feeding pipe mouth of pipe (311) of quartz ampoule (31).
4. a kind of particulate organic carbon according to claim 1, total organic carbon analyzer, it is characterized in that, described low-temperature decomposition reactor (4) includes low-temperature decomposition reactor base (48), be provided with quartz ampoule support (413) in low-temperature decomposition reactor base (48), quartz ampoule support (413) is provided with quartz ampoule (41), end at quartz ampoule (41) is provided with the sample feeding pipe mouth of pipe (411), in quartz ampoule (41), be movably equipped with the sample converyer corresponding to the sample feeding pipe mouth of pipe (411), outside at quartz ampoule (41) other end is provided with cryostat (482), the two ends of quartz ampoule (41) are respectively equipped with carrier gas draft tube (42) and reaction gas escape pipe (43), carrier gas draft tube (42) is communicated with flow controller (18), and reaction gas escape pipe (43) is communicated with condensation hydroextractor (5).
5. a kind of particulate organic carbon according to claim 4, total organic carbon analyzer, it is characterized in that, described sample converyer includes quartz ring (45), be connected with quartz ring connecting rod (451) at quartz ring (45), quartz ring connecting rod (451) is provided with magnetic post (46), be provided with magnet ring track (471) at quartz ampoule support (413), be movably equipped with magnet ring (47) on the magnet ring track (471), magnet ring (47) is corresponding with magnetic post (46), be movably equipped with quartz curette (44) at quartz ring (45), quartz curette (44) is corresponding with the sample feeding pipe mouth of pipe (411) of quartz ampoule (41).
6. a kind of particulate organic carbon according to claim 1, total organic carbon analyzer, it is characterized in that, described conductivity meter (8) comprises conductance cell (81), conductance cell (81) is communicated with respectively base exchanger (82), gas purifier (17) by pipeline, one end of conductance cell (81) is communicated with gas filter (7) by pipeline, the conductance electrode (811) of conductance cell (81) connects electricity by cable and leads controller (80), and electricity is led controller (80) and is connected with data processor (9).
7. a kind of particulate organic carbon according to claim 1, total organic carbon analyzer, it is characterized in that, described conductivity meter (8) comprises conductance cell (81), conductance cell (81) by pipeline be communicated with respectively base reagent (85), electricity is led reactor (83), electricity is led reactor (83) and is communicated with gas purifier (17), one end of conductance cell (81) is communicated with gas filter (7) by pipeline, the conductance electrode (811) of conductance cell (81) connects electricity by cable and leads controller (80), and electricity is led controller (80) and is connected with data processor (9).
CN 201220342506 2012-07-16 2012-07-16 Measuring instrument for particulate organic carbon and total organic carbon Expired - Fee Related CN202661431U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104330526A (en) * 2014-10-13 2015-02-04 成都创源油气技术开发有限公司 Shale organic carbon content analysis simple device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104330526A (en) * 2014-10-13 2015-02-04 成都创源油气技术开发有限公司 Shale organic carbon content analysis simple device
CN104330526B (en) * 2014-10-13 2016-02-03 成都创源油气技术开发有限公司 Shale organic carbon content analyzes easy device

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