CN103940644B

CN103940644B - A kind of front device to saliferous and the Hydrogen-oxygen Isotope test containing organic water

Info

Publication number: CN103940644B
Application number: CN201310025226.2A
Authority: CN
Inventors: 孙维贞; 余海棠; 王瑜; 包诗洁; 张永亮
Original assignee: Cold and Arid Regions Environmental and Engineering Research Institute of CAS
Current assignee: Northwest Institute of Eco Environment and Resources of CAS
Priority date: 2013-01-23
Filing date: 2013-01-23
Publication date: 2016-07-27
Anticipated expiration: 2033-01-23
Also published as: CN103940644A

Abstract

Disclosure is a kind of to the front device of stable hydrogen and oxygen isotopes test in salt water.It is characterized in that guide pin bar is placed on guide pin bar intracavity, be above equipped with pressure pad cap and its spiral connects, pressure pad cap has injection cone mouth, and injection cone mouth connects with carrier gas port, and guide pin bar has vaporization cavity；Guide pin bar puts silica wool bottom chamber；There is heating rod in heating chamber, in temperature control cavity, have temperature probe, heater and temperature probe to connect with Intelligent temperature controller respectively；Insufflation channel upper end connects with blowing nozzle, purges air through insufflation channel and enters the space between earthenware and carbon pipe；Lower end and the sample guide pipe of vapor channel connect, sealing gasket and fixing nut thread connect, and sample guide pipe inserts in the middle of carbon pipe；Being surrounded by silica gel piece outside salt filter, be guard ring outside silica gel piece, whole salt filter is connected by big nut and earthenware spiral are fixing.The present invention completes the mensuration to brackish water, Hydrogen-oxygen Isotope containing organic water sample, the especially mensuration to plateau lake water and arid biogeographic zone river high salinity sample, solves salt and desalts and the problem of organic substance influence.

Description

A kind of front device to saliferous and the Hydrogen-oxygen Isotope test containing organic water

Technical field

The present invention relates to the front device of stable hydrogen and oxygen isotopes test in salt water.

Background technology

In water the research of stable hydrogen and oxygen isotopes at instruction moisture source, explore in Groundwater movement develops and instructs water detection etc. significant, be widely used in the fields such as geoscience, life sciences and atomic energy science.

TCEA method is that grew up in recent years a kind of tests one of new method of Oxygen and Hydrogen isotope ratio in water, it with its cracking completely rapidly, the advantage such as stable, continuous on-line analysis, adopted by domestic and international many laboratorys.But the method is in the mensuration to high salinity samples such as plateau lake water and arid biogeographic zone rivers, and to plant extracts containing in organic sample determination, there are some and insurmountable desalt point and the problem of removing organic substance influence.The present invention is based on the demand, on the basis that many experiments and method improve, and this covering device of Design and Machining, be arranged on the liquid infusion port part of TCEA elemental analyser, be specifically designed to " salt " on-line analysis with organic water sample of desalting.

Summary of the invention

In view of above-mentioned, the purpose of the present invention aims to provide a kind of front device to saliferous and the Hydrogen-oxygen Isotope test containing organic water.This device is directly installed on elemental analyser, it is possible to effectively remove salinity and organic matter in water body.This device decreases the links such as the flowing impact on test result in injection, salting, absorption and carrier gas, has expanded range of application, and stability and the measuring accuracy of analysis are all greatly improved.

The object of the present invention is achieved like this:

A kind of front device to saliferous and the Hydrogen-oxygen Isotope test containing organic water, mainly includes pressure pad cap, guide pin bar, big nut, heater, temperature probe, vaporization chamber, blowing nozzle, sample guide pipe, fixing nut, silica gel piece, guard ring, Intelligent temperature controller, silica wool, injection cone mouth, vapor channel, Carrier carrier gas port, earthenware, carbon pipe, salt filter.Guide pin bar chamber, heater chamber, temperature probe chamber, vapor channel, insufflation channel is had in salt filter；Guide pin bar is placed on guide pin bar intracavity, is above equipped with pressure pad cap and its spiral connects, and pressure pad cap has injection cone mouth, and injection cone mouth connects with carrier gas port, and guide pin bar has vaporization cavity；Guide pin bar puts silica wool bottom chamber；Heating rod, temperature probe intracavity is had to have temperature probe, heater and temperature probe to connect with Intelligent temperature controller respectively in heating chamber；Insufflation channel upper end connects with blowing nozzle, purges air through insufflation channel and enters the space between earthenware and carbon pipe；Lower end and the sample guide pipe of vapor channel connect, sealing gasket and fixing nut thread connect, and sample guide pipe inserts in the middle of carbon pipe；Being surrounded by silica gel piece outside salt filter, be guard ring outside silica gel piece, whole salt filter is connected by big nut and earthenware spiral are fixing.

The invention have the advantage that

The present invention is by brackish water Sample Injection to salt filter, enter (200 DEG C) rapid vaporization in sample vaporization chamber, steam carries lower entrance sample guide pipe at carrier gas stream, is trapped in the silica wool of vaporizer subsequently into entering GC and MS, salinity in water and impurity etc. after example reaction pipe Pintsch process.The advantage of this set salt filter is in that: the 1. salting detention cavity of sample, it is to avoid the carbon pipe caused because of the attachment of salting and the adhesion of earthenware, improves the reaction efficiency of carbon granules；2. radiator valve ensure that the complete rapid vaporization of sample water, reduces memory effect；3. steam is under the delivery of high-purity He, is directly entered the maximum temperature place of carbon reaction tube by downwardly extending sample bar of leading, and reaches the purpose of cracking rapidly completely；4. the Purge air-flow of blowing nozzle, for the backflow of the gases such as CO and the H2 after stopping steam and cracking, reduces memory effect, increases the stability of sample analysis.The principle of the invention is simple, and structure fabrication is exquisite, changes convenient can effectively raising as the important system accessory accuracy for test number, and cost of manufacture is low simultaneously, and long service life has good value for applications.

Accompanying drawing explanation

Fig. 1 is salt filter schematic diagram.

Fig. 2 is this patent guide pin bar figure.

Fig. 3 is this patent salt filter cavity figure.

Below, in conjunction with accompanying drawing, technical scheme is further described again:

As Figure 1-3, a kind of front device to saliferous and the Hydrogen-oxygen Isotope test containing organic water, mainly includes pressure pad cap 1, guide pin bar 2, big nut 3, heater 4, temperature probe 5, vaporization chamber 6, blowing nozzle 7, sample guide pipe 8, fixing nut 9, silica gel piece 10, guard ring 11, Intelligent temperature controller 12, silica wool 14, injection cone mouth 16, Carrier carrier gas port 19, earthenware 20, carbon pipe 21, salt filter 23.Salt filter 23 is contained within guide pin bar chamber 22, heater chamber 15, temperature probe chamber 13, vapor channel 17, insufflation channel 18.Guide pin bar chamber 22 is built-in with guide pin bar 2, guide pin bar 2 top is placed with sealing gasket and threaded by pressure pad cap 1, pressure pad cap 1 has injection cone mouth 16, injection cone mouth 16 connects with the carrier gas port 19 of guide pin bar 2 side, under carrier gas, vapor channel 17 is entered by vaporization chamber 6 after ensureing vaporizing liquid, guide pin bar puts silica wool 14 bottom chamber, is used for filtering salt and grades impurity；Heating rod is put, for vaporization chamber heat temperature raising in heater chamber 15；Temperature probe 5 is placed in temperature probe chamber 13, for testing the temperature of vaporization chamber；Heater 4 and temperature probe 5 are connected with Intelligent temperature controller 12 respectively, arrange temperature controller parameters, maintain vaporization chamber temperature constant；Blowing nozzle 7 connects with insufflation channel 18 upper end helixseal, purge air through insufflation channel 18 and enter the space between earthenware 20 and carbon pipe 21, stop the backflow of the gases such as CO and the H2 after steam flows up and cracks, reduce memory effect, increase the stability of sample analysis；The lower end of sample guide pipe 8 and vapor channel 17 is sealed threaded by fixing nut 9, sample guide pipe 8 is inserted in the middle of carbon pipe 21, length is advisable to reach reaction tube temperature highest point, so makes the steam in passage arrive the maximum temperature reaction zone of carbon pipe 21 smoothly, completes Pintsch process.Being surrounded by silica gel piece 10 outside salt filter 23 for being incubated, be guard ring 11 outside silica gel piece 10, whole salt filter 23 is connected by big nut 3 and earthenware 20 spiral are fixing.

Before sample test, first to carrier gas port 19, blowing nozzle 7, guide pin bar 2, hunt leak respectively in sample guide pipe 8 and big nut 3 threaded connection place, regulate the flow of the two-way helium that elemental analyser is connected with salt filter 23, after Intelligent temperature controller Self-tuning System, set the temperature required vaporization chamber making salt filter heat up, start the intensification leak detection program of elemental analyser TC/EA simultaneously, the rear drive GC/PAL liquid automatic sampler with temperature stabilization is got rid of at gas leakage point, so contain salt and organic water is injected by salt filter pressure pad cap cone mouth 16 after automatic sampler samples, water flows into sample guide pipe 8 with helium after vaporizing in vaporization chamber 6 and enters carbon reaction tube 21 Pintsch process, CO and H2 after cracking is together entered GC and MS and completes the mensuration of hydrogen and oxygen stable isotope ratio by carrier gas.While carrier gas flows into carbon reaction tube Pintsch process, for preventing the backflow of the gas such as CO and H2 after steam and cracking, the Purge air-flow of blowing nozzle 7 problem such as the memory effect that causes of can solving well to reflux.

The use of salt filter 23 is detained substantial amounts of salinity and impurity in vaporization chamber, reduces salting and enters analysis system, first ensure that reaction tube inside and outside wall adheres to without salting, increases the service life；Also reduce the adhesion because the attachment of salting between carbon reaction tube and outermost earthenware occurs；Salting is attached to carbon grain surface simultaneously also affects lysis efficiency；Purge air-flow can prevent gas backstreaming, reduces memory effect, increases the stability of sample test.

Claims

1. the front device to saliferous and the Hydrogen-oxygen Isotope test containing organic water, mainly include earthenware (20), carbon pipe (21) and salt filter (23), salt filter (23) is containing pressure pad cap (1), guide pin bar (2), big nut (3), heater (4), temperature probe (5), vaporization chamber (6), blowing nozzle (7), sample guide pipe (8), fixing nut (9), silica gel piece (10), guard ring (11), Intelligent temperature controller (12), silica wool (14) injection cone mouth (16), Carrier carrier gas port (19), it is characterized in that: salt filter (23) is contained within guide pin bar chamber (22), heater chamber (15), temperature probe chamber (13), vapor channel (17), insufflation channel (18)；Guide pin bar (2) is placed in guide pin bar chamber (22), on be equipped with pressure pad cap (1) and guide pin bar (2) spiral and connect, having injection cone mouth (16) on pressure pad cap (1), injection cone mouth (16) connects with carrier gas port (19), and guide pin bar (2) has vaporization cavity (6)；Silica wool (14) is put bottom guide pin bar chamber；There is heating rod in heater chamber (15), in temperature probe chamber (13), have temperature probe (5), heater (4) and temperature probe (5) to connect with Intelligent temperature controller (12) respectively；Insufflation channel (18) upper end connects with blowing nozzle (7), purges air through insufflation channel (18) and enters the space between earthenware (20) and carbon pipe (21)；Lower end and the sample guide pipe (8) of vapor channel (17) connect, threaded by sealing gasket and fixing nut (9), and sample guide pipe (8) inserts in the middle of carbon pipe (21)；Being surrounded by silica gel piece (10) outside salt filter, be guard ring (11) outside silica gel piece, whole salt filter is connected by big nut (3) and earthenware (20) spiral are fixing.