CN108828083A - The measuring method of releasable volatile organic compounds in luggage - Google Patents

The measuring method of releasable volatile organic compounds in luggage Download PDF

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Publication number
CN108828083A
CN108828083A CN201810368215.7A CN201810368215A CN108828083A CN 108828083 A CN108828083 A CN 108828083A CN 201810368215 A CN201810368215 A CN 201810368215A CN 108828083 A CN108828083 A CN 108828083A
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volatile organic
organic compounds
sampling
temperature
sampler bag
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廖芸
罗峻
朱奕轩
胡剑灿
莫月香
杨欣卉
谢剑飞
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Guangzhou Fiber Product Detects Research Institute
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Guangzhou Fiber Product Detects Research Institute
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present invention relates to a kind of measuring methods of volatile organic compounds releasable in luggage, include the following steps:Sampling:Luggage sample to be measured is fitted into sampler bag, heating discharges the volatile organic compounds in luggage sample to be measured into the sampler bag in 3-6 hours under conditions of temperature is 70 ± 10 DEG C, then is sampled with Tenax-TA sampling pipe to the volatile organic compounds in the sampler bag;Detection:Tenax-TA sampling pipe after sampling is subjected to TDS/GC/MS detection.This method in the case where not destroying sample to be tested can releasable volatile organic compounds in Accurate Determining luggage content, testing cost can be substantially reduced, and economic and environment-friendly.

Description

The measuring method of releasable volatile organic compounds in luggage
Technical field
The present invention relates to technical field of analysis and detection, more particularly to releasable volatile organic compounds in a kind of luggage Measuring method.
Background technique
Volatile organic compounds is a major class source of harmful substance, and the World Health Organization is defined as big in standard Under air pressure, the general name of organic compound of the fusing point lower than room temperature, boiling point lower than 200~260 DEG C.Volatile organic compounds according to Chemical structure, can be divided into alkane, alkene, alkynes, benzene homologues, alcohols, aldehydes, ethers, ketone, acids, esters, halogenated hydrocarbons and its His totally 12 class species, and having virose is mostly benzene homologues and halogenated hydrocarbon.By taking formaldehyde, benzene as an example, long-term contact can be led Cause chronic visceral the dysfunction even generation of cancer;Toluene, dimethylbenzene may generate sense organ (such as eyes or nose) stimulation The respiratory disorder of symptom or asthma class.Luggage may cause volatile organic due to processes such as use, the processing of raw material The residual of object is closed, volatile organic compounds easily can be discharged into environment during use, cause harm to the human body.Luggage makes It is long with human contact's time with frequency is high, to be replaced and cleaned frequency low, if wherein containing harmful substance, must make for a long time At adverse effect, the health and safety of harmful to human.
In luggage relevant industries, the technical requirements standard for being mainly concerned with volatile organic compounds has GB/T 18885- 2009《Ecological textile technical requirements》,GB 19340-2014《Shoes and luggage adhesive》,GB 21550-2008《Polychlorostyrene second Alkene artificial leather limits of harmful substances》, technical requirements quote GB 19340 and GB 21550, such as QB/T in other luggage standards 1333-2010《Carry on the back bag》,QB/T 2155-2010《Luggage》.In these technical requirements standards, GB/T 18885- 2009 are suitable for all kinds of textiles and its attachment, although standard GB/T 18885-2009 gives volatile organic compounds Index, but there is no relevant detection methods.GB 19340 and GB 21550 be respectively suitable for shoes and luggage adhesive and Artificial polyvinyl chloride leather.Band flame ion is used after directly carrying out dissolved dilution to sample using ethyl acetate in standard GB 19340 The gas chromatograph of detector is analyzed, and standard GB 21550 presses method standard GB/T 4615《Polyvinyl chloride residual vinyl chloride The measurement gas chromatography of monomer》Vinyl chloride monomer is measured, sample is dissolved in N, in N '-dimethyl acetamide, using head space Gas chromatography measures the content of vinylchloride in sample.Standard GB/T 24281-2009《The measurement gas of organic volatile compounds in textiles Phase chromatography mass spectrometry》It is also often used in the detection of textile volatile organic compounds, method is clip 100cm2's Sample, with solid phase microextraction (SPME) absorption, measures total organic volatile in gas chromatography-mass spectrum desorption using Head-space sampling instrument Object.Standard SN/T 3587-2013《Import and export the measurement of N,N-dimethylformamide and DMAC N,N' dimethyl acetamide in textile Gas chromatography mass spectrometry method》N,N-dimethylformamide in textile and DMAC N,N' dimethyl acetamide are carried out using solvent-extracted method Test, to be detected after concentration constant volume with GC/MS after the methylene chloride ultrasonic extraction of 20mL × 2.Guangdong Province provincial standard DB44/T 755-2010《The test purge and trap Thermal desorption method of volatile hazardous substances in textile》Sample is cut to 100cm2Area Size is put into scavenging conduit, is had using purge and trap Thermal desorption and Gas chromatographyMass spectrometry to volatility in textile Machine compound carries out qualitative and quantitative analysis.
In existing test method, if all there is following ask in the test for carrying out volatile organic compounds to luggage Topic:It is tested after luggage need to being cut, measuring tank sample packet can be treated and cause irreversible destruction, testing cost is high;And it takes Sample is locality, lacks the total evaluation of sample, cannot reflect truth;Adhesive be luggage class volatile organic matter most Main source, and the adhesive in finished product is difficult to sample;Sample is extracted using organic solvent, the use of organic solvent Harm can be brought to the health and environment of operator.
Summary of the invention
Based on this, the present invention provides a kind of measuring method of volatile organic compounds releasable in luggage, this method Whole-sample can be carried out to luggage, not need to destroy sample, reduce testing cost, and economic and environment-friendly.
Specific technical solution is as follows:
The measuring method of releasable volatile organic compounds, includes the following steps in a kind of luggage:
Sampling:Luggage sample to be measured is fitted into sampler bag, heating makes for 3-6 hours under conditions of temperature is 70 ± 10 DEG C Volatile organic compounds in luggage sample to be measured is discharged into the sampler bag, then is adopted with Tenax-TA sampling pipe to described Volatile organic compounds in sample bag is sampled;
Detection:Tenax-TA sampling pipe after sampling is subjected to TDS/GC/MS detection.
In wherein some embodiments, the sampling includes:Luggage sample to be measured is packed into the sampler bag for being equipped with interface valve In, by the air in sampler bag described in the interface valve nitrogen or inert gas replacement, it is then shut off the interface valve, The sampler bag is sealed;The sampler bag is placed in isoperibol cabin again and carries out heating the volatilization made in luggage sample to be measured Property organic compound discharge into the sampler bag, the temperature of heating is 70 ± 10 DEG C, and the time of heating is 3-6 hours;Then The volatile organic compounds in the sampler bag is sampled by the interface valve with Tenax-TA sampling pipe, was sampled It keeps the sampler bag to be placed in the isoperibol cabin in journey, and the temperature in the isoperibol cabin is kept to add with described The temperature of heat is consistent;After sampling, the interface valve is closed, removes the Tenax-TA sampling pipe and rapidly will be described Tenax-TA samples the seal of tube.
In wherein some embodiments, the temperature of the heating is 70 ± 5 DEG C, and the time of the heating is that 3.5-4.5 is small When.
In wherein some embodiments, the temperature of the heating is 70 ± 2 DEG C, and the time of the heating is 4 hours.
In wherein some embodiments, the volume ratio of the luggage sample to be measured and the sampler bag is 1:1.5-2.5.It takes The sampler bag of the volume ratio is conducive to luggage sample to be measured as the Free up Memory of volatile organic compounds in luggage sample to be measured Volatile organic compounds more complete release under short period and suitable temperature in product, can improve testing result standard While true property, detection efficiency is improved, reduces testing cost.
In wherein some embodiments, when carrying out TDS/GC/MS detection, the parameter of thermal desorption instrument includes:
Desorption temperature:245~255 DEG C;
Desorption time:4~6min;
Throughput is desorbed:28~32mL/min;
Condenser temperature:- 12~-8 DEG C;
Cold hydrazine heating temperature:295~305 DEG C;
Carrier gas:High-purity helium.
In wherein some embodiments, when carrying out TDS/GC/MS detection, gas chromatography-mass spectrum parameter includes:
Chromatographic column:DB-5 (30m × 0.25mm × 0.25 μm) or suitable person;
Injector temperature:245~255 DEG C;
Carrier gas:Nitrogen, 1~1.4mL/min of constant current;
Temperature program:40 DEG C of holding 3min of initial temperature rise to 150 DEG C of holding 2min with 5 DEG C/min, then with 20 DEG C/min 290 DEG C are risen to, 2min is kept;
Transmission line temperature:280℃;
Ionization mode:Electron impact ionization (EI);
Ionizing energy:70eV;
Scanning mode:Full scan mode, ion range 15-500.
In wherein some embodiments, by sampler bag described in the interface valve nitrogen or inert gas replacement Air includes:It is filled with the nitrogen or inert gas of the 25-35% that volume is sampler bag capacity in the sampler bag, then evacuates Gas in the sampler bag, 2~3 times repeatedly;Then 25 ± 2 DEG C at a temperature of to be filled in the sampler bag volume be to adopt The nitrogen or inert gas of the 30-50% of sample bag volume.In order to avoid the volatile organic compounds and air in sampler bag Chemical reaction occurs under the high temperature conditions and causes accuracy that is dangerous and influencing detection, needs the air in sampler bag with lazy Property gas is replaced.Due to expanding with heat and contract with cold, it is filled with excessive inert gas, may result in sampler bag explosion in a heated condition And also it is unfavorable for the release of volatile organic compounds, if the volatility in the very few sample of the amount for being filled with inert gas is organic Compound can also cannot get good release.The inertia of the 30-50% of sampler bag volume is filled with by repeated multiple times experiment discovery Gas flow is than conveniently, being conducive to the release of volatile organic compounds in sample, improving the accuracy of testing result, most preferably It is 40%.
In wherein some embodiments, the Tenax-TA sampling pipe passes through the interface valve in the sampler bag Volatile organic compounds be sampled including:One end of the interface valve of the sampler bag and gas-guide tube is connected, gas-guide tube The other end is equipped with valve and can be connected to the outside in isoperibol cabin, takes out the gas in gas-guide tube in advance with sampling pump, so The valve of gas-guide tube is closed afterwards, then the valvular one end that sets of gas-guide tube is successively connected with Tenax-TA sampling pipe and sampling pump It connects, the valve of the interface valve and the gas-guide tube of opening the sampling pump and the sampler bag is sampled;The Tenax- TA sampling pipe and sampling pump are placed in the outside in the isoperibol cabin, and the temperature in isoperibol face out of my cabin is 25 ± 2 DEG C.
It is 100~200mL/ with the acquisition flow that Tenax-TA sampling pipe is sampled in wherein some embodiments min.The sample to be tested of required volume can be collected faster in the range of flow, if flow velocity is too slow time-consuming, flow velocity is too It will lead to penetrating for object fastly.
In wherein some embodiments, the acquisition volume 0.8-1.2L that is sampled with Tenax-TA sampling pipe.Acquire body The bigger response of product is higher, but it is possible that the case where Tenax-TA pipe overloads, and the time acquired also will increase, The volume of 0.8-1.2L is more suitable.
The measuring method of releasable volatile organic compounds has the following advantages and beneficial effect in luggage of the invention:
The present inventor obtains the releasable volatility in a kind of pair of luggage by the research of a large amount of creative experiments The method that organic compound carries out whole-sample and detected:Sample to be tested is sealed in polyvinyl fluoride sampler bag, is filled with A certain amount of nitrogen or inert gas, then sampler bag is heated at the specified temperature, the after a certain period of time VOC in sample to be tested Component volatilization acquires sampler bag by sampling pump in collection bag, then with Tenax-TA adsorption tube connection sampler bag with constant flow rate In gas, so that the volatile organic compounds component in gas is adsorbed in Tenax-TA trap tube, then recycle Thermal desorption Desorption system is desorbed at high temperature to be sent directly into gas chromatograph-mass spectrometer (GC-MS) and is tested and analyzed, and luggage to be measured can be obtained The content of volatile organic compounds in sample.This method of the invention can be accurate in the case where not destroying sample to be tested The content of the volatile organic compounds discharged in measurement luggage, can substantially reduce testing cost, and be not necessarily in sampling process Any organic solvent is used, it is economic and environment-friendly, and sampling method is whole sampling, avoiding spot sampling in existing method cannot The defect for reflecting truth, substantially increases the reliability and accuracy of testing result.
Detailed description of the invention
Fig. 1 is the test spectrogram result of embodiment 1.
Fig. 2 is influence diagram of the treatment temperature to test result of embodiment 2.
Fig. 3 is influence diagram of the processing time to test result of embodiment 3.
Fig. 4 is that the recovery test in embodiment 4 tests spectrogram.
Specific embodiment
It is done below by way of measuring method of the specific embodiment to volatile organic compounds releasable in luggage of the invention Further details of explanation.
Embodiment 1
The measuring method of releasable volatile organic compounds in a kind of luggage provided in this embodiment, including following step Suddenly:
1. sampling
Sample to be tested in the present embodiment is that blue children carry on the back bag (volume is about 24L), which is packed into 50L body It in long-pending polyvinyl fluoride sampler bag, is sealed with sealing strip, sampler bag is equipped with interface valve.It is filled in the sampler bag for having sample to envelope pure Nitrogen, packing volume are the 30% of sampler bag capacity, then with pump by evacuating air, 2~3 times repeatedly.Then in 25 ± 2 DEG C of ring It is filled with the pure nitrogen gas of 20L at a temperature of border, turns off interface valve, sampler bag is sealed.A blank sampler bag separately is taken, is not put into be measured Sample executes above step, as control.Two sampler bags are placed in 70 ± 2 DEG C of isoperibol cabins and are heated, keep 4 Hour.Simultaneously by the interface valve of one end connection collection bag of gas-guide tube, the other end of gas-guide tube is equipped with valve and can be with perseverance The outside of warm environmental chamber is connected to, and the interface valve of collection bag and the valve of gas-guide tube is kept to be in closing shape in heating process State.
After the completion of heating, valvular one end of setting of gas-guide tube is connected into sampling pump, opens connecing for sampling pump and collection bag The valve of mouth valve and gas-guide tube takes out the gas of 100mL in advance, the interface valve and gas-guide tube of closing sampling pump and collection bag Valve.Gas-guide tube is set into valvular one end successively with Tenax-TA sampling pipe and gas samping pump of flow rate correction again Connection, opens sampling pump and the interface valve of sampler bag and the valve of the gas-guide tube is sampled;Notice that Tenax-TA is adsorbed The installation direction of pipe will meet the gas production direction of adsorption tube requirement.
Sampler bag is kept to be placed in 70 ± 2 DEG C of isoperibol cabin in sampling process, Tenax-TA sampling pipe and sampling pump It is placed in the outside in isoperibol cabin, the temperature in isoperibol face out of my cabin is 25 ± 2 DEG C.Acquisition flow is 100~200mL/ Min, acquisition volume are 1L.After sampling, valve is closed, removes Tenax-TA sampling pipe and rapidly by Tenax-TA sampling pipe Both ends sealing.
Machine testing on 2.
Tenax-TA sampling pipe is subjected to TDS/GC/MS detection and analysis as early as possible, testing conditions are as follows:
The thermal desorption condition of 2.1 setting thermal desorption instruments is as follows
Desorption temperature:250℃;
Desorption time:5min;
Throughput is desorbed:30mL/min;
Condenser temperature:-10℃;
Cold hydrazine heating temperature:300℃;
Carrier gas:High-purity helium.
The testing conditions of 2.2 setting gas chromatography-mass spectrums are as follows:
Chromatographic column:DB-5(30m×0.25mm×0.25μm);
Injector temperature:250℃;
Carrier gas:Nitrogen, purity >=99.999%, constant current 1.2mL/min;
Temperature program:40 DEG C of holding 3min of initial temperature rise to 150 DEG C of holding 2min with 5 DEG C/min, then with 20 DEG C/min 290 DEG C are risen to, 2min is kept;
Input mode:Splitless injecting-Sample;When object overload, changeable split ratio is retested.
Transmission line temperature:280℃;
Ionization mode:Electron impact ionization (EI);
Ionizing energy:70eV;
Scanning mode:Full scan mode, ion range 15-500.
3. the calculating and analysis of testing result
The content of single volatile organic compounds in 3.1 samples:
It is quantified using calibration curve external standard method, the content of single releasable volatile organic compounds passes through in sample Following formula is calculated:
In formula:
CXFor the concentration of the releasable volatile organic compounds of single target in sample, mg/m3
mXFor the quality of the collected single volatile organic compounds of sampling pipe sampled to sample to be tested, mg;
mbFor volatile organic compounds single in the sampling pipe (blank control pipe) that is sampled to blank sampler bag Quality, mg;
V is sampling volume, L;
The conversion coefficient of 0.869 sampling volume volume when being converted to 25 DEG C when being 70 DEG C.
The calculating of volatile organic compounds total amount in 3.2 samples:
All compounds of the retention time between n-hexane (2.39min) and hexadecane (28.38min) are divided Analysis integral, obtains total peak area, is then calculated with the calibration curve of toluene.Sample total volatile organic compounds densimeter Calculation sees below formula:
In formula:
CTFor the total concentration of volatile organic compounds releasable in sample, mg/m3
mTFor the gross mass of the collected volatile organic matter of sampling pipe, mg;
mBFor the gross mass of volatile organic matter in blank tube, mg;
V is sampling volume, L;
The conversion coefficient of 0.869 sampling volume volume when being converted to 25 DEG C when being 70 DEG C.
By test (test spectrogram is shown in Fig. 1), the collected toluene quality of sampling pipe is the sample to be tested of the present embodiment 0.216×10-3Mg, that is, mX=0.216 × 10-3, it is not detected in blank control pipe, sampling volume 1L, i.e. V=1 are updated to It states in formula (1), obtaining releasable concentration of the toluene in sampler bag in sample is 0.249mg/m3.Further according to the concentration and adopt The volume (20L) for the pure nitrogen gas being filled in sample bag can be calculated the amount of releasable toluene in sample to be tested, the present embodiment to The amount that test sample royal blue children carry on the back contained releasable toluene in bag is 0.249mg/m3×0.02m3=0.00498mg=4.98 μ g。
The quality of total volatile organic compounds is 0.223 × 10-3Mg, that is, mT=0.223 × 10-3, blank control Guan Zhongwei Detection, sampling volume 1L, i.e. V=1 are updated in above-mentioned formula (2), are obtained releasable general volatile organic in sample and are closed Concentration C of the object in sampler bagTFor 0.257mg/m3.Further according to the volume (20L) for the pure nitrogen gas being filled in the concentration and sampler bag The amount of releasable total volatile organic compounds in sample to be tested, the sample to be tested blue children back of the present embodiment can be calculated The amount of contained releasable total volatile organic compounds is 0.257mg/m in bag3×0.02m3=0.00514mg=5.14 μ g.
Influence of the 2 sample treatment temperature of embodiment to test result
It is detected according to the method for embodiment 1, only changes the heating temperature in isoperibol cabin, other steps and side Method is the same as embodiment 1.It is respectively adopted 37 DEG C, 60 DEG C, 70 DEG C, 80 DEG C to handle sample to be tested, processing time and implementation Example 1 is identical.Test results are shown in figure 2, the results showed that, temperature is higher, and the burst size of volatile organic compounds is bigger, works as place Release is complete substantially for volatile organic compounds when reason temperature is increased to 70 DEG C;When treatment temperature is 80 DEG C, luggage meeting There is situation of fading, contamination sampling bag comprehensively considers the accuracy of time required for detecting and testing result and do not treat Sample generates destruction, while reducing the consumption of sampler bag, and 70 DEG C are optimal heat treatment temperature.
Influence of 3 sample processing time of embodiment to test result
It is detected according to the method for embodiment 1, only changes the time of the heat treatment in isoperibol cabin, it is other Step and method are the same as embodiment 1.That is middle holding 1h, 2h, 4h and 8h in 70 DEG C of isoperibol cabins respectively by sampler bag.Test As a result as shown in Figure 3, the results showed that:By sample heat time it is longer, the burst size of volatile organic matter is bigger, 4h with The problem of burst size is not further added by substantially afterwards, comprehensively considers detection efficiency and detection accuracy, the heating treatment time of sample are It is optimal selection when 4h.
Embodiment 4
Six kinds of benzene, toluene, ethylbenzene, m- dimethylbenzene, p- dimethylbenzene and o- dimethylbenzene volatile organic compounds are carried out Recovery test (test spectrogram is shown in Fig. 4).Take the standard solution of 500ng/ μ L to Tenax-TA pipe, according to the detection of embodiment 1 Method carries out 6 tests in parallel.Using 3 times of signal-to-noise ratio as detection limit.The rate of recovery, precision, detection limit the results are shown in Table 1, average to return Yield is between 94.1%~102.1%, and precision is between 1.5%~3.8%, as a result accurately and reliably.
1 rate of recovery of table, precision and detection limit
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (10)

1. the measuring method of releasable volatile organic compounds in a kind of luggage, which is characterized in that include the following steps:
Sampling:Luggage sample to be measured is fitted into sampler bag, heating makes to be measured for 3-6 hours under conditions of temperature is 70 ± 10 DEG C Volatile organic compounds in luggage sample is discharged into the sampler bag, then with Tenax-TA sampling pipe to the sampler bag In volatile organic compounds be sampled;
Detection:Tenax-TA sampling pipe after sampling is subjected to TDS/GC/MS detection.
2. the measuring method of releasable volatile organic compounds in luggage according to claim 1, which is characterized in that institute Stating sampling includes:Luggage sample to be measured is fitted into the sampler bag equipped with interface valve, by the interface valve nitrogen or lazy Air in sampler bag described in property gas displacement, is then shut off the interface valve, the sampler bag is sealed;Again by the sampling Bag, which is placed in isoperibol cabin heat, discharges the volatile organic compounds in luggage sample to be measured to the sampler bag In, the temperature of heating is 70 ± 10 DEG C, and the time of heating is 3-6 hours;Then pass through the interface with Tenax-TA sampling pipe Valve is sampled the volatile organic compounds in the sampler bag, and the sampler bag is kept to be placed in the perseverance in sampling process In warm environmental chamber, and keep the temperature in the isoperibol cabin consistent with the temperature of the heating;After sampling, close The interface valve removes the Tenax-TA sampling pipe and the Tenax-TA is sampled the seal of tube rapidly.
3. the measuring method of releasable volatile organic compounds in luggage according to claim 2, which is characterized in that institute The temperature for stating heating is 70 ± 5 DEG C, and the time of the heating is 3.5-4.5 hours.
4. the measuring method of releasable volatile organic compounds in luggage according to claim 3, which is characterized in that institute The temperature for stating heating is 70 ± 2 DEG C, and the time of the heating is 4 hours.
5. the measuring method of releasable volatile organic compounds in luggage according to claim 1-4, special Sign is that when carrying out TDS/GC/MS detection, the parameter of thermal desorption instrument includes:
Desorption temperature:245~255 DEG C;
Desorption time:4~6min;
Throughput is desorbed:28~32mL/min;
Condenser temperature:- 12~-8 DEG C;
Cold hydrazine heating temperature:295~305 DEG C;
Carrier gas:High-purity helium.
6. the measuring method of releasable volatile organic compounds in luggage according to claim 1-4, special Sign is that when carrying out TDS/GC/MS detection, the parameter of gas chromatography-mass spectrum includes:
Chromatographic column:DB-5(30m×0.25mm×0.25μm);
Injector temperature:245~255 DEG C;
Carrier gas:Nitrogen, 1~1.4mL/min of constant current;
Temperature program:40 DEG C of holding 3min of initial temperature are risen to 150 DEG C of holding 2min with 5 DEG C/min, then are risen to 20 DEG C/min 290 DEG C, keep 2min;
Transmission line temperature:280℃;
Ionization mode:Electron impact ionization (EI);
Ionizing energy:70eV;
Scanning mode:Full scan mode, ion range 15-500.
7. special according to the measuring method of volatile organic compounds releasable in the described in any item luggages of claim 2-4 Sign is, includes by the air in sampler bag described in the interface valve nitrogen or inert gas replacement:In the sampling It is filled with the nitrogen or inert gas of the 25-35% that volume is sampler bag capacity in bag, then evacuates the gas in the sampler bag, 2~3 times repeatedly;Then 25 ± 2 DEG C at a temperature of be filled in the sampler bag 30-50%'s that volume is sampler bag volume Nitrogen or inert gas.
8. special according to the measuring method of volatile organic compounds releasable in the described in any item luggages of claim 2-4 Sign is, described to be carried out by the interface valve to the volatile organic compounds in the sampler bag with Tenax-TA sampling pipe Sampling includes:One end of the interface valve of the sampler bag and gas-guide tube is connected, the other end of gas-guide tube is equipped with valve and can To be connected to the outside in isoperibol cabin, the gas in gas-guide tube is taken out in advance with sampling pump, be then shut off the valve of gas-guide tube, then The valvular one end that sets of gas-guide tube is successively connect with Tenax-TA sampling pipe and sampling pump, the sampling pump and described is opened The valve of the interface valve of sampler bag and the gas-guide tube is sampled;The Tenax-TA sampling pipe and sampling pump are placed in institute State the outside in isoperibol cabin, the temperature in isoperibol face out of my cabin is 25 ± 2 DEG C.
9. the measuring method of releasable volatile organic compounds in luggage according to claim 1-3, special Sign is, is 100~200mL/min with the acquisition flow that Tenax-TA sampling pipe is sampled.
10. the measuring method of releasable volatile organic compounds in luggage according to claim 1-3, special Sign is, the acquisition volume 0.8-1.2L being sampled with Tenax-TA sampling pipe.
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CN109596731A (en) * 2018-12-14 2019-04-09 中车长春轨道客车股份有限公司 The pocket type screening method of rail vehicle built-in fitting and material release volatile materials
CN112964802A (en) * 2021-02-09 2021-06-15 西安奕斯伟硅片技术有限公司 Method for testing content of low-boiling-point organic matter in wafer loading box
CN114577960A (en) * 2022-03-16 2022-06-03 中南大学 Cadaveric odor substance collecting device and detection and visual analysis method

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CN112964802A (en) * 2021-02-09 2021-06-15 西安奕斯伟硅片技术有限公司 Method for testing content of low-boiling-point organic matter in wafer loading box
CN114577960A (en) * 2022-03-16 2022-06-03 中南大学 Cadaveric odor substance collecting device and detection and visual analysis method

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Application publication date: 20181116