CN85106189A - A kind of method of measuring trace water in the hydrogen chloride - Google Patents
A kind of method of measuring trace water in the hydrogen chloride Download PDFInfo
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- CN85106189A CN85106189A CN 85106189 CN85106189A CN85106189A CN 85106189 A CN85106189 A CN 85106189A CN 85106189 CN85106189 CN 85106189 CN 85106189 A CN85106189 A CN 85106189A CN 85106189 A CN85106189 A CN 85106189A
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Abstract
The present invention is the method for trace water in a kind of new mensuration hydrogen chloride.Switching by two valves cooperates, and allows tested gas by cold-trap, make hydrogen chloride and moisture from.Analyse by pyrolysis, moisture is identified through electrolytic cell.Because this method has been eliminated the interference of background signal.So can measure the water concentration value that contains 1ppm.This method accuracy height, analysis time lack.Specimen in use is few, and instrument is not produced corrosion.It both can measure trace water in inert gas and the band corrosive gas.Also can be used for carrying out the trace water analysis in the gas of aspects such as semi-conductor industry, nuclear industry, laser, light transmitting fiber and scientific research.
Description
The present invention is a kind of new method of measuring trace moisture content in high-purity hydrogen chloride.
As everyone knows, the method of analyzing liquid water content has a lot, but because water is polar molecule, be easy to be attracted on the wall, pipeline, valve member of analytical instrument, though its quantity seldom, but in accuracy and the exigent trace moisture analysis of degree of accuracy, this interference but is very big, is not easy to ignore.Be that a kind of corrosivity is bigger owing to hydrogen chloride again, the material that chemical property is quite active, this brings bigger difficulty just for the selection and the use of analytical instrument, equipment.In addition, analysis trace water method before, analysis operation time is long, is unfavorable for using.Therefore industrial, in the research document, find that also trace water is less than the analytical approach of the practicality of 10PPM in the mensuration hydrogen chloride.
Analyze the method for trace water in the hydrogen chloride, there have chromatography, CALVER to stop method, current method and dew point method etc. to be several.Document Mioro-Chemical Jonrnal 18 P234～239(1973) the improved CALVER of introduction is stopped method, is more accurate method in the existing method.Its analysis principle is, the hydrogen chloride sample is mixed the cold-trap that causes by dry ice and methyl alcohol, make water condensation get off, that is to say that water is concentrated, and separate with water-free hydrogen chloride gas, put into solvent (pyridine, methyl alcohol) afterwards, condensate water is dissolved, stop the method titration with CALVER again, thereby determine trace water concentration in the hydrogen chloride.
The optimum determining condition of the method is: condenser temperature is between-76-78 ℃; Sample flow rate is below 0.5 liter/minute.Be lower than under the 100PPM condition at the hydrogen chloride water concentration, water can be captured down fully at the condenser pipe place in the hydrogen chloride, and trace water is measured accurately within ± 1PPM.Representative data such as the table 1 measured.
Table 1
The cold calorimetric titration volume of flow velocity sample volume water concentration
(rise/minute) (liter) (℃) (milliliter) (PPM)
0.3 20 -78 1.26 12.6
0.4 20 -78 1.24 12.4
0.5 20 -78 1.28 12.8
0.6 20 -78 1.15 11.5
0.7 21 -78 1.09 10.4
0.8 20 -78 0.94 9.4
0.5 10 -78 0.61 12.1
15 -78 0.98 13.2
20 -78 1.25 12.5
This method Instrument structure as shown in Figure 1.
But this method is stopped reagent and hydrogen chloride and is played the part chemical reaction and influence accuracy owing to CALVER, and under the very low situation of water concentration, error is very big.Solvent and CALVER are stopped water that reagent contains and also the mensuration process are produced and disturb.Solvent and CALVER stop reagent poisonous, flavor is arranged, can produce harm to operating personnel.Again owing to this method mensuration process trouble, so analysis time is long.
The present invention is the method for trace water concentration in a kind of new mensuration hydrogen chloride, and its accuracy is than the additive method height, and analysis time is shorter, and equipment is simple, and specimen in use is few, operates nontoxicly, and analytical instrument is not had corrosion.
Principle of the present invention and method describe in conjunction with apparatus structure synoptic diagram Fig. 2 of the present invention.At first need bioassay standard water curve.The gaseous sample of known water concentration can obtain with the sulfuric acid Bubbling method, and sulfuric acid bubble jar is connected between four-way valve (3) and the six-way valve (4).Six-way valve, adjusting four-way valve and the six-way valve of its six-way valve system through transforming, make high pure nitrogen (2) enter four-way valve by the gas circuit II through clarifier (9), (10), (11), again through sulfuric acid bubbling four, six-way valve by the emptying of gas circuit V, this moment quantity tube (5) be in closure state.Before the condensation quantity tube being put dry ice is cold-trap (6), condensation one minute, rotate six-way valve again, make quantity tube connect sulfuric acid bubble jar, with certain flow rate condensing gas sample, condense to certain hour, promptly, rotate six-way valve, make the high purity nitrogen (2) of purification pass through quantity tube by behind certain volume, take off cold-trap immediately, overlap finish application bath and the aqueous vapor that pyrolysis is come out is brought to electrolytic cell (7),, utilize computing method by pulse water yield signal of register (8) record, make the graph of a relation of pulse area and liquid water content, be the standard water curve.
If the high pure nitrogen of a known aqueous concentration is arranged, can not adopt the sulfuric acid Bubbling method, allow high pure nitrogen directly enter four-way valve by the gas circuit III, adopt and top same measured method, obtain the standard water curve.
The concrete grammar of measuring the unknown gas sample is as follows, earlier with high purity nitrogen (1), each position of purging system.Feed unknown hydrogen chloride gas sample by hydrogen chloride gas sample mouth then, by the gas circuit III, four-way valve, via the emptying of gas circuit IV, again by four-way valve, six-way valve through the emptying of gas circuit V, purify high purity nitrogen (2) pass through quantity tube this moment.During measurement, rotate six-way valve and make the quantity tube sealing, put dry ice and condensation one minute, rotating six-way valve again makes unknown gas sample enter quantity tube, to certain volume, rotate four-way valve with certain flow rate condensing gas sample then, make the purification high pure nitrogen (2) of gas circuit II pass through quantity tube five minutes with 40 ml/min, drive the hydrogen chloride in the quantity tube away, rotate six-way valve again, take off dry ice simultaneously immediately, the cover finish application bath, the moisture content that the pyrolysis condensation is got off is brought the moisture content of pyrolysis into the high purity nitrogen (2) that purifies
Decide device through registering instrument record liquid water content pulse signal.The high purity nitrogen (2) of measuring purification with same procedure is with 40 ml/min, the pulse of the water that is condensed in the nitrogen during by five minutes.With the condensate water pulse area of surveying hydrogen chloride, deduct the pulse area that purifies high purity nitrogen condensate water, the pulse peak area of liquid water content in they poor the has been condensation promptly hydrogen chloride of certain volume, the method can make
Deciding device background undesired signal cancels out each other.Find the corresponding water yield from the standard water curve again, calculate water concentration in the hydrogen chloride gas with following formula:
Wherein: water concentration in the unknown hydrogen chloride of C-
V
aThe water yield (milliliter) of-condensation certain volume hydrogen chloride gas sample
V
2The volume number (milliliter) of the unknown chloro hydrogen of-condensation sample
The method gas velocity is 5～130 ml/min, when condensing temperature is lower than-60 ℃, does not influence condensation efficiency, and under condition of the present invention, cold-trap can will all be caught by moisture content in the gas sample of quantity tube.The operating conditions that is suitable for is: condensing temperature-80 is ℃ to-70 ℃; Gas flow rate 10 ml/min are to 30 ml/min; 150 ℃ to 160 ℃ of thermal desorption temperatures; 105 ℃ to 110 ℃ of pipeline heat insulations.Can analyze the water concentration of moisture 1PPM in the chlorine water hydrogen, survey liquid water content in the high pure nitrogen, with conforming to that the photoelectricity dew point method is surveyed with the method.This method since hydrogen chloride gas without
Decide device, just avoided right
Decide the corrosion of device, and the parts of contact hydrogen chloride can adopt other corrosion-resistant material manufacturings such as stainless steel, glass or teflon.
Practical operation for example Fig. 3, table 2 is listed.Fig. 3 is the standard water curve map.
Table 2
Brief description of drawings.
Fig. 1 is that improved CALVER is stopped method Instrument structure figure.The 1-flowmeter, 2-solvent injection device, 3-cold-trap; 4-titration flask, 5-condenser pipe, 6-sample introduction pipe; 7-electrode sensitive device, 8-stirring rod, 9-teflon protector; the 10-CALVER is stopped the reagent dropper; 11-assists humidity titration flask, and 12,13, the 14-T-valve, the 15-drying tube; the 16-rotary screw, 17, the 18-gas passage.
Fig. 2 is an organigram of the present invention.1,2-high pure nitrogen, 3-four-way valve, 4-six-way valve (being six-way valve), 3-quantity tube, 6-cold-trap and oil bath heater, 7-USI-1 type through transforming
Decide device (electrolytic cell), 8-registering instrument, 9-exsiccator, interior dress silica gel, 10-exsiccator, interior dress molecular sieve, the 11-exsiccator, interior dress phosphorus pentoxide, 12-exsiccator, interior dress silica gel, molecular sieve half and half, the 13-needle valve, 14-flowmeter, 15-surge flask, the 16-absorption bottle, I, II, III, IV, V are the gas passage.
Fig. 3 is the standard water curve map.Horizontal ordinate is the peak area of the condensate water pulse peak that recorded by registering instrument, and ordinate is its corresponding water concentration.
Revisal 85106189
After the preceding revisal of the capable revisal of file name page or leaf
Claims 1 16 7 are as claim 57, as claim 6
Claims (8)
1, the analytical approach of trace water in a kind of new mensuration hydrogen chloride, utilize condensation, enrichment method that trace water condensation in the hydrogen chloride gas is got off, and the hydrogen chloride in the eliminating quantity tube, and then the water yield that is condensed is also analyzed in pyrolysis, it is characterized in that having used two high pure nitrogen gas circuit II and III, by the compounding practice of four-way valve, six-way valve, make the water yield warp that is condensed in the quantity tube
Decide device, registering instrument is determined with pulse singaling.
2, as the compounding practice method of claim 1 described four-way valve and six-way valve, it is characterized in that making earlier water condensation in the hydrogen chloride, separator reheater to separate out, and the background undesired signal of registering instrument record is cancelled out each other, making the background output signal is zero.
3,, it is characterized in that it being through improved six-way valve with common six-way valve as claim 1 described six-way valve.
4, as claim 1 described method, it is characterized in that the pipeline heat insulation temperature is 105 ℃ to 110 ℃, the quantity tube pyrolysis temperature is 150 ℃ to 160 ℃.
5, as claim 1 described method, it is characterized by condensing temperature is-80 ℃ to-70 ℃.
6, as claim 1 described method, it is characterized by, the high pure nitrogen of gas circuit II is with a cover gas cleaning unit.
7,, it is characterized in that exsiccator (9) dress silica gel as claim 5 described purification plants; Exsiccator (10) dress 4A molecular sieve; Exsiccator (11) dress phosphorus pentoxide.
8, as claim 1 described method, it is characterized in that
Decide device and use USI-1 type trace moisture analyzer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85106189 CN85106189A (en) | 1985-08-20 | 1985-08-20 | A kind of method of measuring trace water in the hydrogen chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85106189 CN85106189A (en) | 1985-08-20 | 1985-08-20 | A kind of method of measuring trace water in the hydrogen chloride |
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| CN85106189A true CN85106189A (en) | 1987-04-29 |
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| CN 85106189 Pending CN85106189A (en) | 1985-08-20 | 1985-08-20 | A kind of method of measuring trace water in the hydrogen chloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102445051A (en) * | 2011-10-31 | 2012-05-09 | 绍兴市东湖生化有限公司 | Method for preparing liquid hydrogen chloride form hydrogen chloride gas through compression |
| CN103134875A (en) * | 2011-12-01 | 2013-06-05 | 中国科学院大连化学物理研究所 | On-line pretreatment device of aquatic volatile organic compounds |
-
1985
- 1985-08-20 CN CN 85106189 patent/CN85106189A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102445051A (en) * | 2011-10-31 | 2012-05-09 | 绍兴市东湖生化有限公司 | Method for preparing liquid hydrogen chloride form hydrogen chloride gas through compression |
| CN103134875A (en) * | 2011-12-01 | 2013-06-05 | 中国科学院大连化学物理研究所 | On-line pretreatment device of aquatic volatile organic compounds |
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