Photoelectron-grade ultrapure ammonia process analysis and sampling system and analysis and sampling method

Abstract

The invention discloses a photoelectron-grade ultrapure ammonia process analysis sampling system and a sampling analysis method, the analysis sampling system comprises a process gas analysis system, a carrier gas purification system, a compressed air system and a hydrogen source, the process gas analysis system comprises a first gas chromatographic analysis system, a moisture analysis system, a purging system, a second gas chromatographic analysis system, an evacuation system and a tail gas recovery system. According to the system, the content of each component in the photoelectron-grade ultra-pure ammonia process can be rapidly analyzed by one set of equipment, automatic sampling and analysis can be realized in the whole process, the analysis is accurate, and pollution and waste of the analyzed ultra-pure ammonia gas to the atmosphere are avoided by a tail gas recovery pipeline. The method is high in sampling analysis efficiency, and the sampling process is slightly interfered by external impurities.

Description

Technical Field

[0001] The invention relates to a photoelectronic grade ultrapure ammonia process analysis sampling system and an analysis sampling method. Background Art

[0002] Optoelectronic grade ultra-pure ammonia is one of the key basic chemical materials in the process of manufacturing ultra-large-scale integrated circuits. It is mainly used in chip cleaning, etching, doping and precipitation processes, and has an important impact on the yield, electrical performance and reliability of integrated circuits. With the development of semiconductor industry technology, related industries have higher and higher requirements for the detection level of impurities in optoelectronic grade ultra-pure ammonia, and the expansion of the industry scale has also put forward higher requirements for the improvement of detection efficiency.

[0003] The impurities in optoelectronic grade ultra-pure ammonia mainly include impurities in the air such as nitrogen, oxygen, carbon monoxide, carbon dioxide, and impurities generated by the production process such as methane, ethane, propane and other hydrocarbon substances. In addition, moisture in optoelectronic grade ultra-pure ammonia gas is also a detection item. Different gas chromatographs are required to detect process gases, and different chromatographs have different requirements for carrier gas and drive gas. When the existing analysis technology completes the full component analysis of the process gas, it firstly requires a long time to replace the pipeline and needs to take samples twice respectively, and secondly, it cannot meet the needs of online continuous automatic analysis, and the timeliness and repeatability of the data cannot be guaranteed. Summary of the invention

[0004] The first technical problem to be solved by the present invention is to provide a photoelectronic grade ultra-pure ammonia process analysis sampling system, which can realize a set of equipment to quickly analyze the content of each component in the photoelectronic grade ultra-pure ammonia process, and can realize the process analysis requirements of continuous automatic sampling and analysis, and the analysis is accurate.

[0005] The second technical problem to be solved by the present invention is to provide a method for sampling of photoelectronic grade ultrapure ammonia process analysis, which has high sampling and analysis efficiency and little interference from external impurities during the sampling process.

[0006] In order to solve the problems that the prior art needs to perform gas chromatography and moisture analysis separately when analyzing photoelectron-grade ultra-pure ammonia, the analysis efficiency is low, and insufficient processing during sampling leads to a large relative deviation of the analysis data, the technical solution of the present invention is: a photoelectron-grade ultra-pure ammonia process analysis sampling system, including a process gas analysis system, a carrier gas purification system, a compressed air system and a hydrogen source: (1) The process gas analysis system includes: the first gas chromatography analysis system, the moisture analysis system, the purge system, the second gas chromatography analysis system, the evacuation system, and the tail gas recovery system.

[0007] 1) The first gas chromatography analysis system comprises: a first filter 201, a first pneumatic two-way diaphragm valve 401, a first pressure sensor 1001, a second pressure regulating valve 602, a seventh pneumatic two-way diaphragm valve 407, and a first gas chromatograph 1201 connected in sequence; a pipeline between the first process gas inlet 101 and the first pneumatic two-way diaphragm valve 401 is provided with a first heating belt 301; a pipeline between the first pneumatic two-way diaphragm valve 401 and the first pressure sensor 1001 is provided with a second heating belt 302; a pipeline between the second pressure regulating valve 602 and the seventh pneumatic two-way diaphragm valve 407 is provided with a fourth heating belt 304; and the second pressure regulating valve 602 is provided with a second pressure gauge 702; 2) The moisture analysis system includes: a first pressure regulating valve 601, a third pneumatic two-way diaphragm valve 403, a third filter 203, a seventh manual two-way diaphragm valve 507, and a moisture meter 1301 connected in sequence, the first pressure regulating valve 601 is provided with a first pressure gauge 701, a third heating belt 303 is provided from the first pressure sensor 1001 to the third pneumatic two-way diaphragm valve 403, a fifth heating belt 305 is provided in the pipeline from the third pneumatic two-way diaphragm valve 403 to the seventh manual two-way diaphragm valve 507, and the first pressure regulating valve 601 is connected to the first pressure sensor 1001; 3) The purge system includes: a high-purity nitrogen inlet 1401, an eighth pneumatic two-way diaphragm valve 408, a second filter 202, an eighth pressure regulating valve 608, and a third one-way valve 803 connected in sequence, and then divided into three paths, one path is connected to the first gas chromatography system through the second pneumatic two-way diaphragm valve 402, one path is connected to the second gas chromatography system through the ninth pneumatic two-way diaphragm valve 409, and one path is connected to the moisture analysis system through the ninth pressure regulating valve 609 and the tenth pneumatic two-way diaphragm valve 410. The eighth pressure regulating valve 608 is provided with an eighth pressure gauge 708 and a ninth pressure gauge 709, and the ninth pressure regulating valve 609 is provided with a tenth pressure gauge 710; 4) The second gas chromatography analysis system comprises: a second process gas inlet 102, a fourth filter 204, an eleventh pneumatic two-way diaphragm valve 411, a second pressure sensor 1002, a tenth pressure regulating valve 610, a fifteenth pneumatic two-way diaphragm valve 415, and a second gas chromatograph 1202 connected in sequence, a sixth heating belt 306 being provided on the pipeline between the second process gas inlet 102 and the second pressure sensor 1002, a seventh heating belt 307 being provided on the pipeline between the second pressure sensor 1002 and the tenth pressure regulating valve 610, an eleventh pressure gauge 711 and a twelfth pressure gauge 712 being provided on the tenth pressure regulating valve 610, and an eighth heating belt 308 being provided on the pipeline between the tenth pressure regulating valve 610 and the second gas chromatograph 1202; 5) The evacuation system includes: the second vacuum pump 902 is connected to the pipeline between the second pressure regulating valve 602 and the seventh pneumatic two-way diaphragm valve 407 through the fifth pneumatic two-way diaphragm valve 405, the second vacuum pump 902 is connected to the pipeline between the tenth pressure regulating valve 610 and the fifteenth pneumatic two-way diaphragm valve 415 through the thirteenth pneumatic two-way diaphragm valve 413, and the second vacuum pump 902 is connected to the exhaust gas recovery main pipe through the ninth one-way valve 809; 6) The tail gas recovery system includes: The first gas chromatography system is connected to the tail gas recovery main pipe through the first pressure sensor 1001, the fourth pneumatic two-way diaphragm valve 404, the first non-return valve 801, and the first manual two-way diaphragm valve 501 in sequence; the first gas chromatograph 1201 is connected to the tail gas recovery main pipe through the seventh pneumatic two-way diaphragm valve 407, the sixth pneumatic two-way diaphragm valve 406, and the second non-return valve 802 in sequence; the first gas chromatograph 1201 is connected to the tail gas recovery main pipe through the first flow meter 1101, the fourth non-return valve 804, and the eighth manual two-way diaphragm valve 508 in sequence; the moisture meter 1301 is connected to the tail gas recovery main pipe through the ninth manual two-way diaphragm valve 509, the first vacuum pump 901, the fifth non-return valve 805, The tenth manual two-way diaphragm valve 510 is connected to the exhaust gas recovery main pipe; the second gas chromatography system is connected to the exhaust gas recovery main pipe through the twelfth pneumatic two-way diaphragm valve 412, the eighth one-way valve 808, and the thirteenth manual two-way diaphragm valve 513 in sequence; the second gas chromatography system is connected to the exhaust gas recovery main pipe through the fourteenth pneumatic two-way diaphragm valve 414; the second gas chromatograph 1202 is connected to the exhaust gas recovery main pipe through the second flow meter 1102, the sixth one-way valve 806, and the eleventh manual two-way diaphragm valve 511 in sequence; the second gas chromatograph 1202 is connected to the exhaust gas recovery main pipe through the third flow meter 1103, the seventh one-way valve 807, and the twelfth manual two-way diaphragm valve 512 in sequence.

[0008] (2) The carrier gas purification system includes: the carrier gas source is divided into two paths through the carrier gas inlet 1601: one path passes through the second manual two-way diaphragm valve 502, the third pressure regulating valve 603, and the purifier 1901 and is connected to the first gas chromatograph 1201; the other path passes through the third manual two-way diaphragm valve 503 and the fourth pressure regulating valve 604 in sequence and is connected to the second gas chromatograph 1202; the third pressure regulating valve 603 is provided with a third pressure gauge 703, and the fourth pressure regulating valve 604 is provided with a fourth pressure gauge 704.

[0009] (3) The compressed air system includes: the compressed air is divided into three paths after passing through the compressed air inlet 1801: one path is connected to the first gas chromatograph 1201 through the fourth manual two-way diaphragm valve 504 and the fifth pressure regulating valve 605 in sequence; the second path is connected to the second gas chromatograph 1202 through the fifth manual two-way diaphragm valve 505 and the sixth pressure regulating valve 606 in sequence; the third path is connected to the second gas chromatograph 1202 through the sixth manual two-way diaphragm valve 506 and the seventh pressure regulating valve 607; the fifth pressure regulating valve 605 is provided with a fifth pressure gauge 705, the sixth pressure regulating valve 606 is provided with a sixth pressure gauge 706, and the seventh pressure regulating valve 607 is provided with a seventh pressure gauge 707.

[0010] (4) The hydrogen source 1701 is connected to the second gas chromatograph 1202.

[0011] Furthermore, the moisture meter is preferably a cavity ring-down moisture meter, the first gas chromatograph is preferably a helium discharge ionization gas chromatograph, and the second gas chromatograph is preferably a thermal conductivity or hydrogen flame ionization dual detector gas chromatograph.

[0012] Furthermore, the heating tape is set at a temperature of 50~70°C.

[0013] Furthermore, the entire piping system uses EP grade stainless steel pipes with electropolished inner walls.

[0014] Furthermore, the analysis pipeline connections of the entire pipeline system all adopt the VCR connection method.

[0015] Furthermore, the first pressure sensor 1001 and the fourth pneumatic two-way diaphragm valve 404, and the second pressure sensor 1002 and the twelfth pneumatic two-way diaphragm valve 412 are respectively interlocked. When the first pressure sensor 1001 and the second pressure sensor 1002 reach the set values, the fourth pneumatic two-way diaphragm valve 404 and the twelfth pneumatic two-way diaphragm valve 412 automatically open to release pressure to ensure pipeline safety.

[0016] Furthermore, the first gas chromatography system completes the evacuation replacement and pressure-changing replacement of the pipeline through the fifth pneumatic two-way diaphragm valve 405, the second vacuum pump 902, the sixth pneumatic two-way diaphragm valve 406 and the seventh pneumatic two-way diaphragm valve 407. The second gas chromatography system completes the evacuation replacement and pressure-changing replacement of the pipeline through the thirteenth pneumatic two-way diaphragm valve 413, the second vacuum pump 902, the fourteenth pneumatic two-way diaphragm valve 414 and the fifteenth pneumatic two-way diaphragm valve 415.

[0017] To solve the second technical problem, the present invention provides a method for photoelectronic grade ultrapure ammonia process analysis sampling, comprising the following steps: (1) Evacuate the sampling pipeline: start the second vacuum pump, open the fifth pneumatic two-way diaphragm valve and the thirteenth pneumatic two-way diaphragm valve. After 2 to 3 minutes, when the pressure of the first pressure sensor and the second pressure sensor both display -0.5 ~-1.0 bar, first close the fifth pneumatic two-way diaphragm valve and the thirteenth pneumatic two-way diaphragm valve 413, and then close the second vacuum pump. The pipeline is evacuated.

[0018] (2) Replacement of sampling pipeline: Open the first process gas inlet, the first pneumatic two-way diaphragm valve, and the second pressure regulating valve, and repeatedly open and close the sixth pneumatic two-way diaphragm valve 3 to 5 times, with an opening and closing interval of not less than 5 seconds, to complete the replacement; open the second process gas inlet, the eleventh pneumatic two-way diaphragm valve, and the tenth pressure regulating valve, and repeatedly open and close the fourteenth pneumatic two-way diaphragm valve 3 to 5 times, with an opening and closing interval of not less than 5 seconds, to complete the replacement.

[0019] (3) Sampling and analysis: Open the seventh pneumatic two-way diaphragm valve and the fifteenth pneumatic two-way diaphragm valve respectively, and the test gas enters the first gas chromatograph and the second gas chromatograph for analysis respectively. Open the first pressure regulating valve and adjust the pressure to 0.1~0.4MPa. Open the third pneumatic two-way diaphragm valve, the seventh manual two-way diaphragm valve, the ninth manual two-way diaphragm valve, the first vacuum pump, and the tenth manual two-way diaphragm valve in sequence. The gas from the first process gas inlet starts to enter the moisture meter for moisture analysis. Close the third pneumatic two-way diaphragm valve, open the ninth pneumatic two-way diaphragm valve, open the ninth pressure regulating valve and adjust the pressure to 0.1~0.4MPa. Open the tenth pneumatic two-way diaphragm valve, and the gas from the second process gas inlet starts to enter the moisture meter for moisture analysis.

[0020] (4) End of analysis: Close the first pneumatic two-way diaphragm valve, the second pneumatic two-way diaphragm valve, the third pneumatic two-way diaphragm valve, and the ninth pneumatic two-way diaphragm valve in sequence, and open the eighth pneumatic two-way diaphragm valve, the tenth pneumatic two-way diaphragm valve, the seventh manual two-way diaphragm valve, the ninth manual two-way diaphragm valve, and the tenth manual two-way diaphragm valve in sequence. Continue to purge the moisture analyzer with high-purity nitrogen.

[0021] The sampling system of the present invention can realize N2 or helium purging of the first gas chromatograph, the moisture analyzer, and the second gas chromatograph respectively.

[0022] The sampling system of the present invention has the following characteristics: The present invention provides a sampling method and sampling system for photoelectron-grade ultrapure ammonia process analysis. Compared with the existing analysis technology: each instrument analyzes the impurity components in ultrapure ammonia separately, the present invention can not only realize the full analysis of gas phase impurities and moisture in one injection, but also realize automatic sampling and analysis in the whole process, and the tail gas recovery pipeline avoids the pollution and waste of ultrapure ammonia gas to the atmosphere after analysis. The entire photoelectron-grade ultrapure ammonia process analysis sampling method and sampling system have the advantages of environmental protection, safety, high efficiency and energy saving in the process of analyzing photoelectron-grade ultrapure ammonia, and have great significance in practical application. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 The invention discloses a photoelectronic grade ultra-pure ammonia process analysis sampling system.

[0024] Wherein: 101. First process gas inlet 102. Second process gas inlet 201. First filter 202. Second filter 203. Third filter 204. Fourth filter 301. First heating belt 302. Second heating belt 303. Third heating belt 304. Fourth heating belt 305. Fifth heating belt 306. Sixth heating belt 307. Seventh heating belt 308. Eighth heating belt 401. First pneumatic two-way diaphragm valve 402. Second pneumatic two-way diaphragm valve 403. Third pneumatic two-way diaphragm valve 404. Fourth pneumatic two-way diaphragm valve 405. Fifth pneumatic two-way diaphragm valve 406. Sixth pneumatic two-way diaphragm valve 407. Seventh pneumatic two-way diaphragm valve 408. Eighth pneumatic two-way diaphragm valve 409. Ninth pneumatic two-way Diaphragm valve 410. Tenth pneumatic two-way diaphragm valve 411. Eleventh pneumatic two-way diaphragm valve 412. Twelfth pneumatic two-way diaphragm valve 413. Thirteenth pneumatic two-way diaphragm valve 414. Fourteenth pneumatic two-way diaphragm valve 415. Fifteenth pneumatic two-way diaphragm valve 501. First manual two-way diaphragm valve 502. Second manual two-way diaphragm valve 503. Third manual two-way diaphragm valve 504. Fourth manual two-way diaphragm valve 505. Fifth manual two-way diaphragm valve 506. Sixth manual two-way diaphragm valve 507. Seventh manual two-way diaphragm valve 508. Eighth manual two-way diaphragm valve 509. Ninth manual two-way diaphragm valve 510. Tenth manual two-way diaphragm valve 511. Eleventh manual two-way diaphragm valve 512. Twelfth manual two-way diaphragm valve 513. Thirteenth manual two-way diaphragm valve 601. First pressure regulating valve 602. Second pressure regulating valve 603. Third pressure regulating valve 604. Fourth pressure regulating valve 605. Fifth pressure regulating valve 606. Sixth pressure regulating valve 607. Seventh pressure regulating valve 608. Eighth pressure regulating valve 609. Ninth pressure regulating valve 610. Tenth pressure regulating valve 701. First pressure gauge 702. Second pressure gauge 703. Third pressure gauge 704. Fourth pressure gauge 705. Fifth pressure gauge 706. Sixth pressure gauge 707. Seventh pressure gauge 708. Eighth pressure gauge 709. Ninth pressure gauge 710. Tenth pressure gauge 711. Tenth pressure gauge 712. Second pressure gauge 801. First check valve 802. Second check valve 803. Third check valve 804. Fourth check valve 805. Fifth check valve 806. Sixth check valve 807. Seventh check valve 808. Eighth check valve 809. Ninth check valve 901. First vacuum pump 902. Second vacuum pump 1001. First pressure sensor 1002. Second pressure sensor 1101. First flow meter 1102. Second flow meter 1103. Third flow meter 1201. First gas chromatograph 1202. Second gas chromatograph 1301. Moisture meter 1401. High purity nitrogen inlet 1501.Tail gas recovery main pipe inlet 1601 carrier gas inlet 1701. Hydrogen source 1801. Compressed air inlet 1901. Purifier. DETAILED DESCRIPTION

[0025] To introduce the technical solution provided by the present invention in more detail, it is described below in conjunction with embodiments.

[0026] Example 1

[0027] (1) The process gas analysis system includes: the first gas chromatography analysis system, the moisture analysis system, the purge system, the second gas chromatography analysis system, the evacuation system, and the tail gas recovery system.

[0028] 1) The first gas chromatography analysis system comprises: a first filter 201, a first pneumatic two-way diaphragm valve 401, a first pressure sensor 1001, a second pressure regulating valve 602, a seventh pneumatic two-way diaphragm valve 407, and a first gas chromatograph 1201 connected in sequence; a pipeline between the first process gas inlet 101 and the first pneumatic two-way diaphragm valve 401 is provided with a first heating belt 301; a pipeline between the first pneumatic two-way diaphragm valve 401 and the first pressure sensor 1001 is provided with a second heating belt 302; a pipeline between the second pressure regulating valve 602 and the seventh pneumatic two-way diaphragm valve 407 is provided with a fourth heating belt 304; and the second pressure regulating valve 602 is provided with a second pressure gauge 702; 2) The moisture analysis system includes: a first pressure regulating valve 601, a third pneumatic two-way diaphragm valve 403, a third filter 203, a seventh manual two-way diaphragm valve 507, and a moisture meter 1301 connected in sequence, the first pressure regulating valve 601 is provided with a first pressure gauge 701, a third heating belt 303 is provided from the first pressure sensor 1001 to the third pneumatic two-way diaphragm valve 403, a fifth heating belt 305 is provided in the pipeline from the third pneumatic two-way diaphragm valve 403 to the seventh manual two-way diaphragm valve 507, and the first pressure regulating valve 601 is connected to the first pressure sensor 1001; 3) The purge system includes: a high-purity nitrogen inlet 1401, an eighth pneumatic two-way diaphragm valve 408, a second filter 202, an eighth pressure regulating valve 608, and a third one-way valve 803 connected in sequence, and then divided into three routes, one route is connected to the first gas chromatography system through the second pneumatic two-way diaphragm valve 402, one route is connected to the second gas chromatography system through the ninth pneumatic two-way diaphragm valve 409, and one route is connected to the moisture analysis system through the ninth pressure regulating valve 609 and the tenth pneumatic two-way diaphragm valve 410. The eighth pressure regulating valve 608 is provided with an eighth pressure gauge 708 and a ninth pressure gauge 709, and the ninth pressure regulating valve 609 is provided with a tenth pressure gauge 710. The first gas chromatography system, the second gas chromatography system, and the moisture analysis system are purged respectively; 4) The second gas chromatography analysis system comprises: a second process gas inlet 102, a fourth filter 204, an eleventh pneumatic two-way diaphragm valve 411, a second pressure sensor 1002, a tenth pressure regulating valve 610, a fifteenth pneumatic two-way diaphragm valve 415, and a second gas chromatograph 1202 connected in sequence, a sixth heating belt 306 being provided on the pipeline between the second process gas inlet 102 and the second pressure sensor 1002, a seventh heating belt 307 being provided on the pipeline between the second pressure sensor 1002 and the tenth pressure regulating valve 610, an eleventh pressure gauge 711 and a twelfth pressure gauge 712 being provided on the tenth pressure regulating valve 610, and an eighth heating belt 308 being provided on the pipeline between the tenth pressure regulating valve 610 and the second gas chromatograph 1202; 5) The evacuation system includes: the second vacuum pump 902 is connected to the pipeline between the second pressure regulating valve 602 and the seventh pneumatic two-way diaphragm valve 407 through the fifth pneumatic two-way diaphragm valve 405, the second vacuum pump 902 is connected to the pipeline between the tenth pressure regulating valve 610 and the fifteenth pneumatic two-way diaphragm valve 415 through the thirteenth pneumatic two-way diaphragm valve 413, and the second vacuum pump 902 is connected to the exhaust gas recovery main pipe through the ninth one-way valve 809; 6) The tail gas recovery system includes: The first gas chromatography system is connected to the tail gas recovery main pipe through the first pressure sensor 1001, the fourth pneumatic two-way diaphragm valve 404, the first non-return valve 801, and the first manual two-way diaphragm valve 501 in sequence, which is used for overpressure release of gas in the pipeline; the first gas chromatograph 1201 is connected to the tail gas recovery main pipe through the seventh pneumatic two-way diaphragm valve 407, the sixth pneumatic two-way diaphragm valve 406, and the second non-return valve 802 in sequence, which is used for pipeline gas replacement; the first gas chromatograph 1201 is connected to the tail gas recovery main pipe through the first flowmeter 1101, the fourth non-return valve 804, and the eighth manual two-way diaphragm valve 508 in sequence, so as to realize the collection of the tail gas of the first gas chromatography analysis; the moisture meter 1301 is connected to the tail gas recovery main pipe through the ninth manual two-way diaphragm valve 509, the first vacuum pump 901, the fifth non-return valve 805, the tenth manual two-way The diaphragm valve 510 is connected to the exhaust gas recovery main pipe to realize the collection of exhaust gas analyzed by the moisture meter; the second gas chromatography system is connected to the exhaust gas recovery main pipe through the twelfth pneumatic two-way diaphragm valve 412, the eighth one-way valve 808, and the thirteenth manual two-way diaphragm valve 513 in sequence, which is used for overpressure release of gas in the pipeline; the second gas chromatography system is connected to the exhaust gas recovery main pipe through the fourteenth pneumatic two-way diaphragm valve 414 for pipeline gas replacement; the second gas chromatograph 1202 is connected to the exhaust gas recovery main pipe through the second flowmeter 1102, the sixth one-way valve 806, and the eleventh manual two-way diaphragm valve 511 in sequence; the second gas chromatograph 1202 is connected to the exhaust gas recovery main pipe through the third flowmeter 1103, the seventh one-way valve 807, and the twelfth manual two-way diaphragm valve 512 in sequence, to realize the collection of exhaust gas analyzed by the second gas chromatography.

[0029] (2) The carrier gas purification system includes: the carrier gas source is divided into two paths through the carrier gas inlet 1601: one path passes through the second manual two-way diaphragm valve 502, the third pressure regulating valve 603, and the purifier 1901 and is connected to the first gas chromatograph 1201; the other path passes through the third manual two-way diaphragm valve 503 and the fourth pressure regulating valve 604 in sequence and is connected to the second gas chromatograph 1202; the third pressure regulating valve 603 is provided with a third pressure gauge 703, and the fourth pressure regulating valve 604 is provided with a fourth pressure gauge 704.

[0030] (3) The compressed air system includes: the compressed air is divided into three paths after passing through the compressed air inlet 1801: one path passes through the fourth manual two-way diaphragm valve 504 and the fifth pressure regulating valve 605 in sequence to be connected to the first gas chromatograph 1201; one path passes through the fifth manual two-way diaphragm valve 505 and the sixth pressure regulating valve 606 in sequence to be connected to the second gas chromatograph 1202; the last path is connected to the second gas chromatograph 1202 through the sixth manual two-way diaphragm valve 506 and the seventh pressure regulating valve 607; the fifth pressure regulating valve 605 is provided with a fifth pressure gauge 705, the sixth pressure regulating valve 606 is provided with a sixth pressure gauge 706, and the seventh pressure regulating valve 607 is provided with a seventh pressure gauge 707.

[0031] (4) The hydrogen source 1701 is connected to the second gas chromatograph 1202.

[0032] The moisture meter is preferably a cavity ring-down moisture meter, the first gas chromatograph is preferably a helium discharge ionization gas chromatograph, and the second gas chromatograph is preferably a thermal conductivity and hydrogen flame ionization dual detector gas chromatograph.

[0033] The heating tape is set at a temperature of 50~70℃.

[0034] The entire piping system is made of EP grade stainless steel pipes with electropolished inner walls.

[0035] The analysis pipeline connections of the entire pipeline system all adopt VCR connection method.

[0036] The first pressure sensor 1001 and the fourth pneumatic two-way diaphragm valve 404, and the second pressure sensor 1002 and the twelfth pneumatic two-way diaphragm valve 412 are interlocked respectively. When the first pressure sensor 1001 and the second pressure sensor 1002 reach the set values, the fourth pneumatic two-way diaphragm valve 404 and the twelfth pneumatic two-way diaphragm valve 412 automatically open to release pressure to ensure pipeline safety.

[0037] The first gas chromatography system completes the evacuation replacement and pressure-changing replacement of the pipeline through the fifth pneumatic two-way diaphragm valve 405, the second vacuum pump 902, the sixth pneumatic two-way diaphragm valve 406 and the seventh pneumatic two-way diaphragm valve 407. The second gas chromatography system completes the evacuation replacement and pressure-changing replacement of the pipeline through the thirteenth pneumatic two-way diaphragm valve 413, the second vacuum pump 902, the fourteenth pneumatic two-way diaphragm valve 414 and the fifteenth pneumatic two-way diaphragm valve 415.

[0038] The sampling system operation steps are as follows: (1) Evacuate the sampling pipeline: start the second vacuum pump 902, open the fifth pneumatic two-way diaphragm valve 405 and the thirteenth pneumatic two-way diaphragm valve 413. After 2 minutes, when the pressure of the first pressure sensor 1001 and the first pressure sensor 1002 is displayed as -1.0 bar and is stable, first close the fifth pneumatic two-way diaphragm valve 405 and the thirteenth pneumatic two-way diaphragm valve 413 respectively, and then close the second vacuum pump 902. The pipeline is evacuated.

[0039] (2) Replacement of sampling pipeline: Open the first process gas inlet, the first pneumatic two-way diaphragm valve 401, and the second pressure regulating valve 602, and repeatedly open and close the sixth pneumatic two-way diaphragm valve 406 five times, with an opening and closing interval of 7 seconds, to complete the replacement. Open the second process gas inlet 102, the eleventh pneumatic two-way diaphragm valve 411, and the tenth pressure regulating valve 610, and repeatedly open and close the fourteenth pneumatic two-way diaphragm valve 414 five times, with an opening and closing interval of 7 seconds, to complete the replacement.

[0040] (3) Sampling and analysis: Open the seventh pneumatic two-way diaphragm valve 407 and the fifteenth pneumatic two-way diaphragm valve 415 respectively, and the gas to be tested enters the first gas chromatograph 1201 and the second gas chromatograph 1202 for analysis respectively. Open the first pressure regulating valve and adjust the pressure to 0.1~0.4MPa, open the third pneumatic two-way diaphragm valve 403, the seventh manual two-way diaphragm valve 507, the ninth manual two-way diaphragm valve 509, the first vacuum pump 901, and the tenth manual two-way diaphragm valve 510 in sequence, and the gas from the first process gas inlet starts to enter the moisture meter for moisture analysis. Close the third pneumatic two-way diaphragm valve 403, open the ninth pneumatic two-way diaphragm valve 409, open the ninth pressure regulating valve 609 and adjust the pressure to 0.1~0.4MPa, open the tenth pneumatic two-way diaphragm valve 410, and the gas from the second process gas inlet starts to enter the moisture meter for moisture analysis.

[0041] (4) End of analysis: close the first pneumatic two-way diaphragm valve 401, the second pneumatic two-way diaphragm valve 402, the third pneumatic two-way diaphragm valve 403, and the ninth pneumatic two-way diaphragm valve 409 in sequence, and open the eighth pneumatic two-way diaphragm valve 408, the tenth pneumatic two-way diaphragm valve 410, the seventh manual two-way diaphragm valve 507, the ninth manual two-way diaphragm valve 509, and the tenth manual two-way diaphragm valve 510 in sequence, so that high-purity nitrogen gas can continue to purge the moisture analyzer.

[0042] The analysis sampling system of the present invention is used to simultaneously analyze the moisture and air components in industrial ammonia. The entire analysis time is 10 minutes. The methane content is measured to be 1849.28 ppm, the ethane content is 0.14 ppm, the propane content is 0.014 ppm, and the moisture content is 0.1 ppm. The relative standard deviation of the analysis data of three repeated analyses is less than 3%. The analysis process is efficient and the data accuracy is high.

[0043] In summary, the sampling system and method of the present invention solve the problems in the prior art that gas chromatography and moisture analysis need to be performed separately when analyzing optoelectronic grade ultra-pure ammonia, the analysis efficiency is low, and insufficient processing during sampling leads to a large relative deviation of the analysis data. The system and method of the present invention are easy to operate and accurate in analysis, and can be applied to the effective monitoring of various impurity components during the continuous production of optoelectronic grade ultra-pure ammonia.

Claims

1. A photoelectronic grade ultra-pure ammonia process analysis sampling system, including a process gas analysis system, a carrier gas purification system, a compressed air system and a hydrogen source: (1) The process gas analysis system includes: The first gas chromatography analysis system, the moisture analysis system, the purge system, the second gas chromatography analysis system, the evacuation system, and the tail gas recovery system; 1) A first gas chromatography analysis system comprises: a first filter (201), a first pneumatic two-way diaphragm valve (401), a first pressure sensor (1001), a second pressure regulating valve (602), a seventh pneumatic two-way diaphragm valve (407), and a first gas chromatograph (1201) which are connected in sequence; a first heating belt (301) is provided in the pipeline between the first process gas inlet (101) and the first pneumatic two-way diaphragm valve (401); a second heating belt (302) is provided in the pipeline between the first pneumatic two-way diaphragm valve (401) and the first pressure sensor (1001); a fourth heating belt (304) is provided in the pipeline between the second pressure regulating valve (602) and the seventh pneumatic two-way diaphragm valve (407); and the second pressure regulating valve (602) is provided with a second pressure gauge (702); 2) The moisture analysis system comprises: a first pressure regulating valve (601), a third pneumatic two-way diaphragm valve (403), a third filter (203), a seventh manual two-way diaphragm valve (507), and a moisture meter (1301) connected in sequence, the first pressure regulating valve (601) being provided with a first pressure gauge (701), a third heating belt (303) being provided from the first pressure sensor (1001) to the third pneumatic two-way diaphragm valve (403), a fifth heating belt (305) being provided in a pipeline from the third pneumatic two-way diaphragm valve (403) to the seventh manual two-way diaphragm valve (507), and the first pressure regulating valve (601) being connected to the first pressure sensor (1001); 3) The purge system comprises: a high-purity nitrogen inlet (1401), an eighth pneumatic two-way diaphragm valve (408), a second filter (202), an eighth pressure regulating valve (608), and a third one-way valve (803) connected in sequence, and then divided into three paths, one path connected to the first gas chromatography system through the second pneumatic two-way diaphragm valve (402), one path connected to the second gas chromatography system through the ninth pneumatic two-way diaphragm valve (409), and one path connected to the moisture analysis system through the ninth pressure regulating valve (609) and the tenth pneumatic two-way diaphragm valve (410), the eighth pressure regulating valve (608) being provided with an eighth pressure gauge (708) and a ninth pressure gauge (709), and the ninth pressure regulating valve (609) being provided with a tenth pressure gauge (710); 4) The second gas chromatography analysis system comprises: a second process gas inlet (102), a fourth filter (204), an eleventh pneumatic two-way diaphragm valve (411), a second pressure sensor (1002), a tenth pressure regulating valve (610), a fifteenth pneumatic two-way diaphragm valve (415), and a second gas chromatograph (1202) connected in sequence, the pipeline between the second process gas inlet (102) and the second pressure sensor (1002) being provided with a sixth heating belt (306), the pipeline between the second pressure sensor (1002) and the tenth pressure regulating valve (610) being provided with a seventh heating belt (307), the tenth pressure regulating valve (610) being provided with an eleventh pressure gauge (711) and a twelfth pressure gauge (712), and the pipeline between the tenth pressure regulating valve (610) and the second gas chromatograph (1202) being provided with an eighth heating belt (308); 5) The evacuation system comprises: the second vacuum pump (902) is connected to the pipeline between the second pressure regulating valve (602) and the seventh pneumatic two-way diaphragm valve (407) through the fifth pneumatic two-way diaphragm valve (405), the second vacuum pump (902) is connected to the pipeline between the tenth pressure regulating valve (610) and the fifteenth pneumatic two-way diaphragm valve (415) through the thirteenth pneumatic two-way diaphragm valve (413), and the second vacuum pump (902) is connected to the exhaust gas recovery main pipe through the ninth one-way valve (809); 6) The tail gas recovery system includes: the first gas chromatography system is connected to the tail gas recovery main pipe through the first pressure sensor (1001), the fourth pneumatic two-way diaphragm valve (404), the first non-return valve (801), and the first manual two-way diaphragm valve (501) in sequence; the first gas chromatograph (1201) is connected to the tail gas recovery main pipe through the seventh pneumatic two-way diaphragm valve (407), the sixth pneumatic two-way diaphragm valve (406), and the second non-return valve (802) in sequence; the first gas chromatograph (1201) is connected to the tail gas recovery main pipe through the first flow meter (1101), the fourth non-return valve (804), and the eighth manual two-way diaphragm valve (508) in sequence; the moisture meter (1301) is connected to the tail gas recovery main pipe through the ninth manual two-way diaphragm valve (509), the first vacuum pump (901), the fifth non-return valve (80 5), the tenth manual two-way diaphragm valve (510) is connected to the exhaust gas recovery main pipe; the second gas chromatography system is connected to the exhaust gas recovery main pipe through the twelfth pneumatic two-way diaphragm valve (412), the eighth one-way valve (808), and the thirteenth manual two-way diaphragm valve (513) in sequence; the second gas chromatography system is connected to the exhaust gas recovery main pipe through the fourteenth pneumatic two-way diaphragm valve (414); the second gas chromatograph (1202) is connected to the exhaust gas recovery main pipe through the second flow meter (1102), the sixth one-way valve (806), and the eleventh manual two-way diaphragm valve (511) in sequence; the second gas chromatograph (1202) is connected to the exhaust gas recovery main pipe through the third flow meter (1103), the seventh one-way valve (807), and the twelfth manual two-way diaphragm valve (512) in sequence; (2) A carrier gas purification system comprises: a carrier gas source is divided into two paths through a carrier gas inlet (1601): one path is connected to a first gas chromatograph (1201) after passing through a second manual two-way diaphragm valve (502), a third pressure regulating valve (603), and a purifier (1901); and the other path is connected to a second gas chromatograph (1202) after passing through a third manual two-way diaphragm valve (503) and a fourth pressure regulating valve (604) in sequence, wherein the third pressure regulating valve (603) is provided with a third pressure gauge (703), and the fourth pressure regulating valve (604) is provided with a fourth pressure gauge (704); (3) The compressed air system comprises: the compressed air is divided into three paths after passing through the compressed air inlet (1801): one path is connected to the first gas chromatograph (1201) through the fourth manual two-way diaphragm valve (504) and the fifth pressure regulating valve (605) in sequence; the second path is connected to the second gas chromatograph (1202) through the fifth manual two-way diaphragm valve (505) and the sixth pressure regulating valve (606) in sequence; the third path is connected to the second gas chromatograph (1202) through the sixth manual two-way diaphragm valve (506) and the seventh pressure regulating valve (607); the fifth pressure regulating valve (605) is provided with a fifth pressure gauge (705), the sixth pressure regulating valve (606) is provided with a sixth pressure gauge (706), and the seventh pressure regulating valve (607) is provided with a seventh pressure gauge (707); (4) The hydrogen source (1701) is connected to the second gas chromatograph (1202).

2. The photoelectronic grade ultrapure ammonia process analysis sampling system according to claim 1 is characterized in that: The moisture meter is a cavity ring-down moisture meter.

3. The photoelectronic grade ultrapure ammonia process analysis sampling system according to claim 1 is characterized in that: The first gas chromatograph is a helium discharge ionization gas chromatograph.

4. The photoelectronic grade ultrapure ammonia process analysis sampling system according to claim 1 is characterized in that: The second gas chromatograph is a thermal conductivity or hydrogen flame ionization dual-detector gas chromatograph.

5. The photoelectronic grade ultrapure ammonia process analysis sampling system according to claim 1 is characterized in that: The entire piping system is made of EP grade stainless steel pipes with electropolished inner walls.

6. The photoelectronic grade ultrapure ammonia process analysis sampling system according to claim 1 is characterized in that: The analysis pipeline connections of the entire pipeline system all adopt VCR connection method.

7. The photoelectronic grade ultrapure ammonia process analysis sampling system according to claim 1 is characterized in that: The first pressure sensor (1001) and the fourth pneumatic two-way diaphragm valve (404) are interlocked.

8. The photoelectronic grade ultrapure ammonia process analysis sampling system according to claim 1 is characterized in that: The second pressure sensor (1002) and the twelfth pneumatic two-way diaphragm valve (412) are interlocked respectively.

9. An analytical sampling method for a photoelectron grade ultrapure ammonia process analytical sampling system according to any one of claims 1 to 8, comprising the following steps: (1) Evacuate the sampling pipeline: start the second vacuum pump, open the fifth pneumatic two-way diaphragm valve and the thirteenth pneumatic two-way diaphragm valve. After 2 to 3 minutes, when the pressure of the first pressure sensor and the second pressure sensor both display -0.5 to -1.0 bar, first close the fifth pneumatic two-way diaphragm valve and the thirteenth pneumatic two-way diaphragm valve 413, and then close the second vacuum pump. The pipeline is evacuated. (2) Replace the sampling pipeline: open the first process gas inlet, the first pneumatic two-way diaphragm valve, and the second pressure regulating valve, and repeatedly open and close the sixth pneumatic two-way diaphragm valve 3 to 5 times, with an opening and closing interval of not less than 5 seconds, to complete the replacement; open the second process gas inlet, the eleventh pneumatic two-way diaphragm valve, and the tenth pressure regulating valve, and repeatedly open and close the fourteenth pneumatic two-way diaphragm valve 3 to 5 times, with an opening and closing interval of not less than 5 seconds, to complete the replacement; (3) Sampling and analysis: Open the seventh pneumatic two-way diaphragm valve and the fifteenth pneumatic two-way diaphragm valve respectively, and the gas to be tested enters the first gas chromatograph and the second gas chromatograph for analysis respectively. Open the first pressure regulating valve and adjust the pressure to 0.1~0.4MPa. Open the third pneumatic two-way diaphragm valve, the seventh manual two-way diaphragm valve, the ninth manual two-way diaphragm valve, the first vacuum pump, and the tenth manual two-way diaphragm valve in sequence. The gas from the first process gas inlet starts to enter the moisture meter for moisture analysis. Close the third pneumatic two-way diaphragm valve, open the ninth pneumatic two-way diaphragm valve, open the ninth pressure regulating valve and adjust the pressure to 0.1~0.4MPa. Open the tenth pneumatic two-way diaphragm valve, and the gas from the second process gas inlet starts to enter the moisture meter for moisture analysis. (4) End of analysis: Close the first pneumatic two-way diaphragm valve, the second pneumatic two-way diaphragm valve, the third pneumatic two-way diaphragm valve, and the ninth pneumatic two-way diaphragm valve in sequence, and open the eighth pneumatic two-way diaphragm valve, the tenth pneumatic two-way diaphragm valve, the seventh manual two-way diaphragm valve, the ninth manual two-way diaphragm valve, and the tenth manual two-way diaphragm valve in sequence. Continue to purge the moisture analyzer with high-purity nitrogen.

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