CN105738491A - Method for detecting carbon tetrachloride content in gas - Google Patents
Method for detecting carbon tetrachloride content in gas Download PDFInfo
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Abstract
The invention discloses a method for detecting a carbon tetrachloride content in gas. The method is used for detecting a carbon tetrachloride content in a to-be-detected gas sample. The method comprises the following steps: detecting a liquid carbon tetrachloride standard sample through a gas chromatographic method and drawing a carbon tetrachloride standard work curve; detecting the to-be-detected gas sample through a gas chromatographic method, and performing contrast with the carbon tetrachloride standard work curve to obtain the carbon tetrachloride mass in the to-be-detected gas sample; and calculating the carbon tetrachloride content in the to-be-detected gas sample. According to the method, quantitative analysis of the carbon tetrachloride content in gas can be accurately and simply carried out.
Description
Technical field
The present invention relates to a kind of analysis method for gases, particularly to the quantitative analysis method of carbon tetrachloride content in a kind of gas.
Background technology
Report to some extent about the quantitative analysis method of carbon tetrachloride content in solid, patent CN10163955A " a kind of analysis method of content of carbon tetrachloride in solid sample " adopts gas chromatography, by the method adding internal standard substance, set up the standard curve of carbon tetrachloride, measure the carbon tetrachloride content in sample, however it is necessary that addition internal standard substance, complicated operation；In patent CN104062390A " chloroform in chlorinated polypropylene, the detection method of carbon tetrachloride and content assaying method ", by setting up the standard curve of carbon tetrachloride, by two kinds of solvents upon solids sample treatment, adopt the content of carbon tetrachloride, complicated operation in gas chromatography detection fluid sample；" gas chromatography of chlorinated paraffin-70 carbon tetrachloride content quickly detects " adopts gas chromatography, by setting up carbon tetrachloride standard curve, measures the content of carbon tetrachloride in liquid；Patent US2004003654A1 adopt liquid chromatography and infrared spectroscopic determination measure the method for each component content in medium.
And it is little about the report of the quantitative approach of carbon tetrachloride content in gas, the conventional method that those skilled in the art adopt is generally using gas gas as standard specimen, method disclosed in the F-HZ-HJ-DQ-0002 mensuration gas chromatography of carbon tetrachloride content " the surrounding air chloroform, ", is namely adopt gas gas as standard specimen.
But, owing to carbon tetrachloride boiling point is higher, prepare gas gas not easily homogeneous gasification, the accuracy of standard specimen own is difficult to ensure that, linear relationship is poor, causes that gaseous sample result evaluated error is relatively big, and method used in the prior art can not obtain good testing result.Therefore, how to set up a kind of method of carbon tetrachloride content in simplicity, practical test gas, make it can carry out the mensuration of carbon tetrachloride content in gas accurately, to realize the analysis of carbon tetrachloride content in gas, namely become those skilled in the art's problem demanding prompt solution.
Summary of the invention
The present invention seeks to be in that providing a kind of tests the method for carbon tetrachloride content in gas so that it is the quantitative analysis carrying out gas carbon tetrachloride content that can be accurate, easy.
For achieving the above object, the present invention provides a kind of and tests the method for carbon tetrachloride content in gas, and for measuring the carbon tetrachloride content in a gaseous sample to be measured, the method comprises the following steps:
1) with gas chromatography test liquid carbon tetrachloride standard specimen, carbon tetrachloride standard working curve is made；
2) test described gaseous sample to be measured with gas chromatography, compare step 1) gained carbon tetrachloride standard working curve, obtain the carbon tetrachloride quality in described gaseous sample to be measured；
3) carbon tetrachloride content obtaining in described gaseous sample to be measured is calculated.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, the liquid carbon tetrachloride standard specimen of preparation gradient concentration, and with gas chromatography, it is tested respectively, in each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains described carbon tetrachloride standard working curve.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, the liquid carbon tetrachloride standard specimen of described gradient concentration is prepared with methanol for solvent.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, the liquid carbon tetrachloride standard specimen of described gradient concentration, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, and standard specimen number is be more than or equal to 5, it is advantageous to be 5～8.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, the order liquid carbon tetrachloride standard specimen of described gradient concentration tested with gas chromatography is for standard specimen concentration from small to large.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, adopting gas chromatograph to test, test condition is: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 200 DEG C～280 DEG C, split ratio 50:1～20:1, column temperature 90 DEG C～120 DEG C, detector temperature 250 DEG C～280 DEG C；Gas sampling amount is 0.1mL～5mL, and Liquid sample introduction amount is 0.5 μ L～5 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, adopting gas chromatograph to test, test condition is preferably: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 250 DEG C, split ratio 30:1, column temperature 100 DEG C, detector temperature 260 DEG C；Gas sampling amount is 3mL, and Liquid sample introduction amount is 2 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 2) in, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, with the abscissa carbon tetrachloride quality of its correspondence, then at step 3) in calculate the carbon tetrachloride content obtaining in described gaseous sample to be measured.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 2) in, adopting gas chromatograph to test, test condition is: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 200 DEG C～280 DEG C, split ratio 50:1～20:1, column temperature 90 DEG C～120 DEG C, detector temperature 250 DEG C～280 DEG C；Gas sampling amount is 0.1mL～5mL, and Liquid sample introduction amount is 0.5 μ L～5 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 2) in, adopting gas chromatograph to test, test condition is preferably: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 250 DEG C, split ratio 30:1, column temperature 100 DEG C, detector temperature 260 DEG C；Gas sampling amount is 3mL, and Liquid sample introduction amount is 2 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 3) in, the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
Compared with prior art, the know-why of the present invention and technique effect thereof are as follows:
1) present invention is the quality utilizing gas chromatogram hydrogen flame detector response value to be proportional in the unit interval component and enter detector, peak area is directly proportional to quality, by liquid standard specimen carbon tetrachloride quality and the quality comparation of carbon tetrachloride in gas, convert through volume, record the content of carbon tetrachloride in gaseous sample.
2) method of the carbon tetrachloride content in test gas provided by the present invention, simple to operate, quick and precisely, practical, it is adaptable to the quantitative analysis of the gaseous sample containing carbon tetrachloride composition.
Describe the present invention below in conjunction with the drawings and specific embodiments, but not as a limitation of the invention.
Accompanying drawing explanation
Fig. 1 be the present invention test gas in the method step flow chart of carbon tetrachloride content；
Fig. 2 is according to the carbon tetrachloride standard working curve obtained by method of carbon tetrachloride content in the test gas of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is described in detail, and what listed illustrative embodiments was only used as to illustrate, it is not intended as the restriction of the present invention.
Refer to Fig. 1, its be the present invention test gas in the method step flow chart of carbon tetrachloride content.For the quantitative analysis carrying out gas carbon tetrachloride content that can be accurate, easy, the present invention provides a kind of and tests the method for carbon tetrachloride content in gas, and for measuring the carbon tetrachloride content in a gaseous sample to be measured, the method comprises the following steps:
1) with gas chromatography test liquid carbon tetrachloride standard specimen, carbon tetrachloride standard working curve is made；
2) test described gaseous sample to be measured with gas chromatography, compare step 1) gained carbon tetrachloride standard working curve, obtain the carbon tetrachloride quality in described gaseous sample to be measured；
3) carbon tetrachloride content obtaining in described gaseous sample to be measured is calculated.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, first the liquid carbon tetrachloride standard specimen of gradient concentration is prepared, then with gas chromatography, the liquid carbon tetrachloride standard specimen of gradient concentration is tested respectively, in each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains described carbon tetrachloride standard working curve.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, the liquid carbon tetrachloride standard specimen of described gradient concentration is prepared with methanol for solvent.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, the liquid carbon tetrachloride standard specimen of described gradient concentration, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, and standard specimen number is be more than or equal to 5, but the preparation of liquid standard specimen is not with described herein for restriction, those skilled in the art can make one's options according to practical situation, it is possible to is 5～8.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, the order liquid carbon tetrachloride standard specimen of described gradient concentration tested with gas chromatography is for standard specimen concentration from small to large.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, adopting gas chromatograph to test, test condition is: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 200 DEG C～280 DEG C, split ratio 50:1～20:1, column temperature 90 DEG C～120 DEG C, detector temperature 250 DEG C～280 DEG C；Gas sampling amount is 0.1mL～5mL, and Liquid sample introduction amount is 0.5 μ L～5 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 1) in, adopting gas chromatograph to test, test condition is preferably: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 250 DEG C, split ratio 30:1, column temperature 100 DEG C, detector temperature 260 DEG C；Gas sampling amount is 3mL, and Liquid sample introduction amount is 2 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 2) in, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, with the abscissa carbon tetrachloride quality of its correspondence, then at step 3) in calculate the carbon tetrachloride content obtaining in described gaseous sample to be measured.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 2) in, adopting gas chromatograph to test, test condition is: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 200 DEG C～280 DEG C, split ratio 50:1～20:1, column temperature 90 DEG C～120 DEG C, detector temperature 250 DEG C～280 DEG C；Gas sampling amount is 0.1m～5mL, and Liquid sample introduction amount is 0.5 μ L～5 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 2) in, adopting gas chromatograph to test, test condition is preferably: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 250 DEG C, split ratio 30:1, column temperature 100 DEG C, detector temperature 260 DEG C；Gas sampling amount is 3mL, and Liquid sample introduction amount is 2 μ L.
Wherein, in the test gas of the present invention in method one better embodiment of carbon tetrachloride content, in step 3) in, the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
Embodiment a
The present embodiment provides a kind of and tests the method for carbon tetrachloride content in gas, for measuring the carbon tetrachloride content in a gaseous sample to be measured, comprises the following steps:
1) liquid carbon tetrachloride standard specimen (the liquid carbon tetrachloride standard specimen of described gradient concentration of gradient concentration is prepared with methanol for solvent, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, standard specimen number is 8), and with gas chromatography, it is tested (order of test is for standard specimen concentration from small to large) respectively, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 200 DEG C, split ratio 50:1, column temperature 90 DEG C, detector temperature 250 DEG C, Liquid sample introduction amount is 0.5 μ L；In each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains carbon tetrachloride standard working curve；
2) described gaseous sample to be measured is tested with gas chromatography, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 200 DEG C, split ratio 50:1, column temperature 90 DEG C, detector temperature 250 DEG C, gas sampling amount is 0.1mL；Comparison step 1) gained carbon tetrachloride standard working curve, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, obtains the carbon tetrachloride quality in described gaseous sample to be measured with the abscissa carbon tetrachloride quality of its correspondence；
3) calculating the carbon tetrachloride content obtaining in described gaseous sample to be measured, computational methods are the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
Embodiment b
The present embodiment provides a kind of and tests the method for carbon tetrachloride content in gas, for measuring the carbon tetrachloride content in a gaseous sample to be measured, comprises the following steps:
1) liquid carbon tetrachloride standard specimen (the liquid carbon tetrachloride standard specimen of described gradient concentration of gradient concentration is prepared with methanol for solvent, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, standard specimen number is 5), and with gas chromatography, it is tested (order of test is for standard specimen concentration from small to large) respectively, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 280 DEG C, split ratio 20:1, column temperature 120 DEG C, detector temperature 280 DEG C, Liquid sample introduction amount is 5 μ L；In each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains carbon tetrachloride standard working curve；
2) described gaseous sample to be measured is tested with gas chromatography, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 280 DEG C, split ratio 20:1, column temperature 120 DEG C, detector temperature 280 DEG C, gas sampling amount is 5mL；Comparison step 1) gained carbon tetrachloride standard working curve, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, obtains the carbon tetrachloride quality in described gaseous sample to be measured with the abscissa carbon tetrachloride quality of its correspondence；
3) calculating the carbon tetrachloride content obtaining in described gaseous sample to be measured, computational methods are the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
Embodiment c
The present embodiment provides a kind of and tests the method for carbon tetrachloride content in gas, for measuring the carbon tetrachloride content in a gaseous sample to be measured, comprises the following steps:
1) liquid carbon tetrachloride standard specimen (the liquid carbon tetrachloride standard specimen of described gradient concentration of gradient concentration is prepared with methanol for solvent, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, standard specimen number is 8), and with gas chromatography, it is tested (order of test is for standard specimen concentration from small to large) respectively, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 230 DEG C, split ratio 40:1, column temperature 95 DEG C, detector temperature 255 DEG C, Liquid sample introduction amount is 1 μ L；In each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains carbon tetrachloride standard working curve；
2) described gaseous sample to be measured is tested with gas chromatography, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 230 DEG C, split ratio 40:1, column temperature 95 DEG C, detector temperature 255 DEG C, gas sampling amount is 1.5mL；Comparison step 1) gained carbon tetrachloride standard working curve, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, obtains the carbon tetrachloride quality in described gaseous sample to be measured with the abscissa carbon tetrachloride quality of its correspondence；
3) calculating the carbon tetrachloride content obtaining in described gaseous sample to be measured, computational methods are the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
Embodiment d
The present embodiment provides a kind of and tests the method for carbon tetrachloride content in gas, for measuring the carbon tetrachloride content in a gaseous sample to be measured, comprises the following steps:
1) liquid carbon tetrachloride standard specimen (the liquid carbon tetrachloride standard specimen of described gradient concentration of gradient concentration is prepared with methanol for solvent, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, standard specimen number is 6), and with gas chromatography, it is tested (order of test is for standard specimen concentration from small to large) respectively, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 260 DEG C, split ratio 25:1, column temperature 110 DEG C, detector temperature 270 DEG C, Liquid sample introduction amount is 3.5 μ L；In each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains carbon tetrachloride standard working curve；
2) described gaseous sample to be measured is tested with gas chromatography, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 260 DEG C, split ratio 25:1, column temperature 110 DEG C, detector temperature 270 DEG C, gas sampling amount is 4mL；Comparison step 1) gained carbon tetrachloride standard working curve, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, obtains the carbon tetrachloride quality in described gaseous sample to be measured with the abscissa carbon tetrachloride quality of its correspondence；
3) calculating the carbon tetrachloride content obtaining in described gaseous sample to be measured, computational methods are the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
Embodiment e
The present embodiment provides a kind of and tests the method for carbon tetrachloride content in gas, for measuring the carbon tetrachloride content in a gaseous sample to be measured, comprises the following steps:
1) liquid carbon tetrachloride standard specimen (the liquid carbon tetrachloride standard specimen of described gradient concentration of gradient concentration is prepared with methanol for solvent, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, standard specimen number is 7), and with gas chromatography, it is tested (order of test is for standard specimen concentration from small to large) respectively, test condition is: have the gas chromatograph of hydrogen flame detector, chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 250 DEG C, split ratio 30:1, column temperature 100 DEG C, detector temperature 260 DEG C；Liquid sample introduction amount is 2 μ L；In each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains carbon tetrachloride standard working curve；
2) testing described gaseous sample to be measured with gas chromatography, test condition is: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 (60m × 0.32mm × 1.0 μm) capillary column, gasification temperature 250 DEG C, split ratio 30:1, column temperature 100 DEG C, detector temperature 260 DEG C；Gas sampling amount is 3mL；Comparison step 1) gained carbon tetrachloride standard working curve, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, obtains the carbon tetrachloride quality in described gaseous sample to be measured with the abscissa carbon tetrachloride quality of its correspondence；
3) calculating the carbon tetrachloride content obtaining in described gaseous sample to be measured, computational methods are the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
Compared with prior art, the know-why of the present invention and technique effect thereof are as follows:
1) present invention is the quality utilizing gas chromatogram hydrogen flame detector response value to be proportional in the unit interval component and enter detector, peak area is directly proportional to quality, by liquid standard specimen carbon tetrachloride quality and the quality comparation of carbon tetrachloride in gas, convert through volume, record the content of carbon tetrachloride in gaseous sample.
2) method of the carbon tetrachloride content in test gas provided by the present invention, simple to operate, quick and precisely, practical, it is adaptable to the quantitative analysis of the gaseous sample containing carbon tetrachloride composition.
By the examples below and experimental data the method for carbon tetrachloride content in the test gas of the present invention is described further, to clearly show that its technique effect.
1, experimental principle
Gas chromatogram hydrogen flame detector is mass flow rate sensitive detector, and its response value is proportional in the unit interval component and enters the quality of detector.Injecting the liquid carbon tetrachloride standard specimen of certain volume accordingly, corresponding to gaseous sample, with the relation of quality Yu peak area, calculating the quality of carbon tetrachloride in certain sample size gas, thus recording the content of carbon tetrachloride in gaseous sample.
2, key instrument and reagent
Agilent7890 gas chromatograph (Agilent company of the U.S.)；
Carbon tetrachloride, analytical pure；
Containing carbon tetrachloride gas (calcium carbide factory of Jilin Petrochemical company)；
Electronic balance
3, experimental technique
3.1, the preparation of liquid standard specimen and gas gas
Liquid standard specimen is prepared: prepare the carbon tetrachloride liquid standard specimen of different content in penicillin bottle with methanol for solvent.
Gas gas: in 100mL syringe, with air for carrier gas, injects a certain amount of liquid carbon tetrachloride, the carbon tetrachloride gas gas of preparation different content.
3.2, GC conditions
7890A gas chromatograph, HP-1 (60m × 0.32mm × 1.0 μm) capillary column, fid detector；Gasification temperature 280 DEG C, split ratio 20:1, column temperature 120 DEG C, detector temperature 280 DEG C；Sample size: gas 100 μ L, liquid 1 μ L.
3.3, the drafting of carbon tetrachloride standard curve
Refer to Fig. 2, it is with above-mentioned GC conditions, the carbon tetrachloride liquid standard specimen of the gradient concentration of preparation is measured, this curve of carbon tetrachloride standard curve then drawn is with the quality of carbon tetrachloride for abscissa, the corresponding carbon tetrachloride liquid standard working curve that peak area is vertical coordinate.
Additionally, again with above-mentioned GC conditions, the carbon tetrachloride gas gas of the gradient concentration of preparation is measured, then draw carbon tetrachloride standard curve, this curve is with the quality of carbon tetrachloride for abscissa, the corresponding carbon tetrachloride gas standard working curve (gas working curve is not shown) that peak area is vertical coordinate.
3.4, the accuracy of method
The accuracy of method is embodied by gas gas and liquid standard specimen Comparative result.
Table 1 gas gas sample introduction quality and peak area corresponding relation and response value
Table 2 liquid standard specimen sample introduction quality and peak area corresponding relation and response value
Gas gas correlation coefficient: r=0.9596；Liquid standard specimen correlation coefficient: r=0.9959.
Response value 11.4 in gas gas, hence it is evident that higher, processes as outlier, and it is 8.12 that calculating obtains average response value, and liquid standard specimen meansigma methods response value is 8.07, then be as the criterion with gas gas, and the relative error of liquid standard specimen and gas gas response value is 0.7%.
Say from relative error, not only feasible as standard specimen with liquid carbon tetrachloride, and also linear relationship is substantially better than gas carbon tetrachloride gas.
3.5, the precision of method
Under selected experiment condition, same sample carrying out 6 times and measures, and use carbon tetrachloride liquid standard working curve to calculate, its relative standard deviation is 9.6%, refers to table 3.
Table 3 Precision Experiment
Certainly; the present invention also can have other various embodiments; when without departing substantially from present invention spirit and essence thereof, those of ordinary skill in the art can make various corresponding change and deformation according to the present invention, but these change accordingly and deform the protection domain that all should belong to the claims in the present invention.
Claims (9)
1. test a method for carbon tetrachloride content in gas, for measuring the carbon tetrachloride content in a gaseous sample to be measured, it is characterised in that the method comprises the following steps:
1) with gas chromatography test liquid carbon tetrachloride standard specimen, carbon tetrachloride standard working curve is made；
2) test described gaseous sample to be measured with gas chromatography, compare step 1) gained carbon tetrachloride standard working curve, obtain the carbon tetrachloride quality in described gaseous sample to be measured；
3) carbon tetrachloride content obtaining in described gaseous sample to be measured is calculated.
2. the method for carbon tetrachloride content in test gas according to claim 1, it is characterized in that, in step 1) in, the liquid carbon tetrachloride standard specimen of preparation gradient concentration, and with gas chromatography, it is tested respectively, in each liquid carbon tetrachloride standard specimen, carbon tetrachloride quality is for abscissa, with each liquid carbon tetrachloride standard specimen peak area of recording for vertical coordinate, draws and obtains described carbon tetrachloride standard working curve.
3. the method for carbon tetrachloride content in test gas according to claim 2, it is characterised in that in step 1) in, the liquid carbon tetrachloride standard specimen of described gradient concentration is prepared with methanol for solvent.
4. the method for carbon tetrachloride content in test gas according to claim 2, it is characterized in that, in step 1) in, the liquid carbon tetrachloride standard specimen of described gradient concentration, carbon tetrachloride quality contained by it is incremented by between 3 μ g～18 μ g, and standard specimen number is be more than or equal to 5.
5. the method for carbon tetrachloride content in test gas according to claim 2, it is characterised in that in step 1) in, the order liquid carbon tetrachloride standard specimen of described gradient concentration tested with gas chromatography is for standard specimen concentration from small to large.
6. the method for carbon tetrachloride content in test gas according to claim 1 and 2, it is characterized in that, in step 1) in, adopting gas chromatograph to test, test condition is: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 capillary column, gasification temperature 200 DEG C～280 DEG C, split ratio 50:1～20:1, column temperature 90 DEG C～120 DEG C, detector temperature 250 DEG C～280 DEG C；Liquid sample introduction amount is 0.5 μ L～5 μ L；HP-1 capillary column specification is 60m × 0.32mm × 1.0 μm.
7. the method for carbon tetrachloride content in test gas according to claim 1, it is characterized in that, in step 2) in, the gaseous sample peak area to be measured recorded is substituted in described carbon tetrachloride standard working curve vertical coordinate peak area, with the abscissa carbon tetrachloride quality of its correspondence, then at step 3) in calculate the carbon tetrachloride content obtaining in described gaseous sample to be measured.
8. the method for carbon tetrachloride content in the test gas according to claim 1 or 7, it is characterized in that, in step 2) in, adopting gas chromatograph to test, test condition is: have the gas chromatograph of hydrogen flame detector, and chromatographic column is HP-1 capillary column, gasification temperature 200 DEG C～280 DEG C, split ratio 50:1～20:1, column temperature 90 DEG C～120 DEG C, detector temperature 250 DEG C～280 DEG C；Gas sampling amount is 0.1mL～5mL；HP-1 capillary column specification is 60m × 0.32mm × 1.0 μm.
9. the method for carbon tetrachloride content in test gas according to claim 1, it is characterised in that in step 3) in, the carbon tetrachloride content=step 2 in described gaseous sample to be measured) gained carbon tetrachloride quality/gaseous sample gross mass to be measured.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020239054A1 (en) * | 2019-05-30 | 2020-12-03 | 特丰制药有限公司 | Method for determining chloralkane content in chloral hydrate or preparation thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603955A (en) * | 2009-07-20 | 2009-12-16 | 中国蓝星（集团）股份有限公司 | The analytical approach of carbon tetrachloride content in a kind of solid sample |
| CN104062390A (en) * | 2014-06-27 | 2014-09-24 | 泸州北方化学工业有限公司 | Method of detecting trichloromethane and carbon tetrachloride in chlorinated polypropylene and method for measuring contents of trichloromethane and carbon tetrachloride in chlorinated polypropylene |
-
2014
- 2014-12-10 CN CN201410753098.8A patent/CN105738491A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603955A (en) * | 2009-07-20 | 2009-12-16 | 中国蓝星（集团）股份有限公司 | The analytical approach of carbon tetrachloride content in a kind of solid sample |
| CN104062390A (en) * | 2014-06-27 | 2014-09-24 | 泸州北方化学工业有限公司 | Method of detecting trichloromethane and carbon tetrachloride in chlorinated polypropylene and method for measuring contents of trichloromethane and carbon tetrachloride in chlorinated polypropylene |
Non-Patent Citations (4)
| Title |
|---|
| I. PAPAEFSTATHIOU等: "Hyphenated pervaporation-solid-phase preconcentration-gas chromatography for the determination of volatile organic compounds in solid samples", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 李亮: "热脱附-气相色谱-质谱法测定环境空气中5种挥发性卤代烃", 《环境科学与管理》 * |
| 潘春颖等: "空气中四氯化碳的热解吸气相色谱测定法研究", 《中国航天医药杂志》 * |
| 舒黎晔等: "毛细管气相色谱法同时测定工作场所空气中的 16种有毒物质", 《中国卫生检验杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020239054A1 (en) * | 2019-05-30 | 2020-12-03 | 特丰制药有限公司 | Method for determining chloralkane content in chloral hydrate or preparation thereof |
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