CN105181942A - Textile formaldehyde content sealed cabin test method - Google Patents
Textile formaldehyde content sealed cabin test method Download PDFInfo
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- CN105181942A CN105181942A CN201510391099.7A CN201510391099A CN105181942A CN 105181942 A CN105181942 A CN 105181942A CN 201510391099 A CN201510391099 A CN 201510391099A CN 105181942 A CN105181942 A CN 105181942A
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Abstract
The invention discloses a textile formaldehyde content sealed cabin test method. The method is a nondestructive detection method, does not cause any damage to textiles, and is applicable to detection of samples and ready-made clothes. At the same time, pump suction formaldehyde air detector testing equipment is employed to detect the acquired steam, thus being able to acquire experimental data in real time, and avoiding the tedious work and test error brought about by follow-up acetylacetone color developing determination and absorbance involved in the traditional standard. The method can acquire a reliable detection result, and has the characteristics of high efficiency, low energy consumption, and suitability for industrial use, etc.
Description
Technical field
The present invention relates to a kind of textile inspection technology, specifically a kind of formaldehyde content of textiles pressurized capsule method of testing.
Background technology
Formaldehyde (HCHO) has another name called formaldehyde, and be a kind of gas of colourless, irritant smell, it belongs to high volatile organic compound, the highly volatile when room temperature, and some formaldehyde effusion during liquid formaldehyde evaporation, great majority change trioxymethylene into.
Formaldehyde is regarded as carcinogenic and teratogen by U.S. environment protection mechanism and the World Health Organization (WHO) (WorldHealthOrganization), is generally acknowledged allergen.Because formaldehyde low price, reaction are active, be widely used weaving, food, building materials etc. and live closely bound up field with us.Free formaldehyde in these materials and release formaldehyde, can bring and serious harm our healthy after Long contact time.It mainly contains following aspect to the harm of health:
A. to the harm of sensorium
Formaldehyde is the most responsive to the stimulation of eyes, and certain density formaldehyde can make eyes stung, redness, shed tears.Textile directly contacts with human body skin, and its formaldehyde contained is more direct to the injury of skin.Formaldehyde is a kind of environment sensibiligen, can cause allergic dermatitis, color spot, even cutaneous necrosis.Because formaldehyde is soluble in water, it is melted into blood rapidly through after skin, along with each position being recycled to intelligent's body of blood, causes significant damage to human body.
B. to the harm of respiratory system
In textile production and process, some auxiliary agent can discharge a large amount of gas formaldehydes.After inhaled formaldehyde, it has strong impulse effect to respiratory apparatus such as nose, throat, bronchuses, causes cough, throat discomfort, sneezes, even can cause the symptom such as sphagitis, bronchial spasm, lung's discomfort.Researchist is to being in concentration of formaldehyde 0.07mg/m
3or the children of higher concentration environment study, found that concentration of formaldehyde is at 0.07mg/m
3or more Gao Shike causes respiratory tract light inflammation.As can be seen here, associated production enterprise must take corresponding safeguard measure that the concentration of formaldehyde is reduced to below safety line, protects that employee's is healthy with this.
C. to the harm of metabolism and excretory system
Formaldehyde in textile, by after entering human body with skin contact or respiratory system, destroys vascular endothelial cell, causes endovascular damage; Protein bound in addition in itself and blood forms irreversible formaldehyde protein cross compound, produces protein precipitation and Mottling formation, causes artery to be hardened.
D. to neural harm
Formaldehyde has neurotoxicity.Find after deliberation, too much Formaldehyde Exposed can cause nervous system downright bad, and RNA, DNA synthesize minimizing.Formaldehyde enters fast transition formic acid after blood, and formaldehyde causes cerebrospinal fluid circulation disorder thus causes cerebral anoxia, and anoxic causes again body acidosis, make cerebral vasodilators, acetin calcium ion enters cell, and in lysosome, a large amount of enzyme of release, finally causes neuronal death.The neurobehaviorals such as by carrying out neurobehavioral function to the workman of Formaldehyde Exposed, scientific research personnel finds that low concentration formaldehyde can affect the notice of people, memory, visual sense are known, perceive motion speed and hands movement velocity accuracy.
E. to reproductive system and hereditary harm
The performance of formaldehyde to arrenotoky endocrine function and sperm has harmful effect.Also certain influence is existed for female fecundity, even causes fetal anomaly.Formaldehyde is as carcinogenic and teratogen, and it can be covalently bonded on DNA and cause DNA damage, gene mutation or chromosome breakage, even suppresses DNA to repair by destroying genome.At present, the harm of formaldehyde to reproduction heredity causes paying close attention to of people, and this is not only related to, and we are healthy, also have tremendous influence to the procreation of people.
" assay method (acetylacetone method) of formaldehyde in textile content " has been drafted by China as far back as 1975, and gets the nod in 1976, as the method for inspection of externally providing a certificate.In the world, Japan is applied to textile finishing operation formaldehyde at first, is also find that formaldehyde has harmfulness to human body the earliest.Japanese health ministry issued 112 decrees in 1974, and the content of this decree to different textile Free-formaldehyde limits respectively.At present, the examination criteria of formaldehyde content of textiles mainly can be divided three classes in the world: aqueous extraction method, vapor absorption method and high performance liquid chromatography.The standard of aqueous extraction method detection formaldehyde mainly contains the GB/T2912.1-2009 " the mensuration Part I of textile formaldehyde: the formaldehyde (aqueous extraction method) dissociating and be hydrolyzed " of China, the examination criteria ISO14184-1 " the mensuration part 1 of textile formaldehyde: free and hydrolysis formaldehyde (aqueous extraction method) " of (European Union) existing detection formaldehyde content of textiles and Japanese JISL1041:2000 " method of testing through resin finishing textile " in the world, aqueous extraction method is at a certain temperature with after distilled water extraction certain hour by the sample of certain mass, with developer, extract is developed the color, and by the absorbance of spectrophotometer measurement nitrite ion, formaldehyde in textile content is calculated finally by formaldehyde standard solution working curve.The method is convenient and swift, simply easy, be widely used in the detection of reality, but it is easily subject to that textile fades, the interference of the factor such as impurity in extract, test result is easily influenced, China GB/T2912.2-2009 " the mensuration Part II of textile formaldehyde: the formaldehyde (vapor absorption method) of release ", the AATCC112 " closed container method measures the release of formaldehyde in fabric " that ISO14184-2 " the mensuration part 2 of textile formaldehyde: free formaldehyde (vapor absorption method) " and U.S. textile chemist and association of printing and dyeing man formulate adopts vapor absorption method to measure content of formaldehyde in textile, the method is at closed container overhung sample, container bottom adds a certain proportion of distilled water, after long-time heated at constant temperature, the distilled water of extraction in evacuation container, developed the color by the formaldehyde absorbed distilled water and measure its absorbance, finally calculate the content of formaldehyde in this sample, this method avoid the impact of impurity in " aqueous extraction method " extract, there is the advantage that the factor of being disturbed is few, but heated at constant temperature 20h, experimental period is longer, energy resource consumption is larger, the method is not suitable for real work and test data is higher, GB/T2912.3-2009 " the mensuration Part III of textile formaldehyde: high performance liquid chromatography ", the method is developed voluntarily by China, water intaking extraction and the process of vapor absorption method after distilled water, with 2,4-dinitrophenylhydrazine is derivatization reagent, generates 2,4-dinitrophenylhydrazone, measure by HPLC-UV detection device (HPLC/UVD) or diode array detector (HPLC/DAD), the content of formaldehyde in last reference standard working curve calculation sample.The method is lower than the detection limit of first two method, not by the interference of impurity in extract, but due to apparatus expensive, maintenance cost high, do not popularized in reality detects.
The detection method of above formaldehyde content of textiles is destructive detection, causes irreversible damage, cause a large amount of textiles to be wasted to textile; And during sampling be on certain position on clip sample or multiple position a fritter test, test result can not represent the content of formaldehyde of one integral piece textile.
Summary of the invention
For overcoming the shortcoming of method of testing in existing standard, the technical matters that quasi-solution of the present invention is determined is: provide a kind of formaldehyde content of textiles pressurized capsule method of testing.The method is Non-Destructive Testing, can not cause any destruction, be applicable to the detection of sample and ready-made clothes to textile, easy to operate, reliable test result.
The technical scheme that the present invention solve the technical problem is: design a kind of formaldehyde content of textiles pressurized capsule method of testing, the method adopts following step:
1) sample is put into pressurized capsule, then pressurized capsule is put into constant temperature oven, by rubber hose, the air intake opening of pump suction type formaldehyde air detection instrument and gas outlet are linked into pressurized capsule inside respectively;
2) temperature 50 C of constant temperature oven is set, treats that temperature rises to 50 DEG C and heated at constant temperature 8h ~ 10h; In this process, the formaldehyde contained in sample just can be released slowly into pressurized capsule inside, and inner for the pressurized capsule gas with formaldehyde flows back and forth by pump suction type formaldehyde air detection instrument between its detection place and pressurized capsule;
3) observe the reading of pump suction type formaldehyde air detection instrument, after stable reading, directly read formaldehyde content values and record, detecting and namely come to an end;
4) by 3) in the formaldehyde content values that reads be converted into the weight content value of sample, namely the data value in units of mg/Kg, and substituted in formula y=2.98741x-6.50991 or y=3.10375x+11.03532 and calculate, show that the value of y is the final formaldehyde content values of sample.
Described formaldehyde content of textiles pressurized capsule method of testing, it is further characterized in that the method adopts following equipment:
Comprise pressurized capsule, constant temperature oven and pump suction type formaldehyde air detection instrument, described pressurized capsule is complete seal cavity, only stays two small through hole for connecting pump suction type formaldehyde air detection instrument; Described two small through hole are positioned at the not coplanar of pressurized capsule or the both sides of the same face; The air intake opening of described pump suction type formaldehyde air detection instrument is connected with two small through hole of pressurized capsule by rubber hose respectively with gas outlet, forms steam circuit; Described constant temperature oven is transformed on commercially available a conventional oven, and design increase by two small sized pipelines can for inserting rubber hose.
Compared with prior art, beneficial effect of the present invention is: adopt pump suction type formaldehyde air detection instrument checkout equipment to detecting containing formaldehyde vapor of collecting, experimental data can be obtained in real time, avoid the tedious work that follow-up its absorbance of diacetone chromogenic assay involved in standard is brought.The present invention can obtain testing result comparatively reliably, has that efficiency is high, energy consumption is low, be suitable for the features such as industrialization use.
Accompanying drawing explanation
Fig. 1 be a kind of embodiment of formaldehyde content of textiles pressurized capsule method of testing of the present invention time PARA FORMALDEHYDE PRILLS(91,95) release affect data analysis figure.
Fig. 2 be a kind of embodiment of formaldehyde content of textiles pressurized capsule method of testing of the present invention temperature PARA FORMALDEHYDE PRILLS(91,95) release affect data analysis figure.
Fig. 3 is the how many impact on testing result of sample content of formaldehyde of a kind of embodiment of formaldehyde content of textiles pressurized capsule method of testing of the present invention.
Fig. 4 is that the testing result of a kind of embodiment of formaldehyde content of textiles pressurized capsule method of testing of the present invention and national standard detect aqueous extraction method testing result linear fit curve.
Fig. 5 is testing result and the national standard vapor absorption method testing result linear fit curve of a kind of embodiment of formaldehyde content of textiles pressurized capsule method of testing of the present invention.
Embodiment
Below by way of test example, content of the present invention is explained:
Specific experiment and experimental data can make the present invention of the art personnel comprehend below, but do not limit the present invention in any way.
A kind of formaldehyde content of textiles pressurized capsule of the present invention method of testing, is characterized in that the method adopts following step:
1) sample is put into pressurized capsule, then pressurized capsule is put into constant temperature oven, by rubber hose, the air intake opening of pump suction type formaldehyde air detection instrument and gas outlet are linked into pressurized capsule inside respectively;
2) temperature 50 C of constant temperature oven is set, treats that temperature rises to 50 DEG C and heated at constant temperature 8h ~ 10h; In this process, the formaldehyde contained in sample just can be released slowly into pressurized capsule inside, and inner for the pressurized capsule gas with formaldehyde flows back and forth by pump suction type formaldehyde air detection instrument between its detection place and pressurized capsule;
3) observe the reading of pump suction type formaldehyde air detection instrument, after stable reading, directly read formaldehyde content values and record, detecting and namely come to an end;
4) by 3) in the formaldehyde content values that reads be converted into the weight content value of sample, namely the data value in units of mg/Kg, and substituted in formula y=2.98741x-6.50991 or y=3.10375x+11.03532 and calculate, show that the value of y is the final formaldehyde content values of sample.
Concrete conversion process is as follows:
The volumetric concentration of formaldehyde content values is converted to mass concentration:
In formula:
Formaldehyde mass concentration in X-pressurized capsule, unit is mg/m
3;
Formaldehyde volumetric concentration in M-pressurized capsule, unit is PPM;
A-formaldehyde molecule quality;
Air molar volume under 22.4-standard state.
The content of formaldehyde in pressurized capsule can be learnt by X value, utilize formula (2) to calculate the content of formaldehyde in sample:
In formula:
The content of formaldehyde extracted in F-sample, unit is mg/Kg;
The mass concentration of formaldehyde in X-pressurized capsule, unit is mg/m
3;
The inner volume of V-pressurized capsule, unit is m
3;
The quality of m-sample, unit is Kg.
Make x=F, and substituted in formula y=2.98741x-6.50991 or y=3.10375x+11.03532 and calculate, show that the value of y is the final formaldehyde content values of sample.
Described formaldehyde content of textiles pressurized capsule method of testing, it is further characterized in that the method adopts following equipment:
Comprise pressurized capsule, constant temperature oven and pump suction type formaldehyde air detection instrument, described pressurized capsule is complete seal cavity, only stays two small through hole for connecting pump suction type formaldehyde air detection instrument; Described two small through hole are positioned at the not coplanar of pressurized capsule or the both sides of the same face; The air intake opening of described pump suction type formaldehyde air detection instrument is connected with two small through hole of pressurized capsule by rubber hose respectively with gas outlet, forms steam circuit; Described constant temperature oven is transformed on commercially available a conventional oven, and design increase by two small sized pipelines can for inserting rubber hose.Pump suction type formaldehyde air detection instrument is commercially available POT400-CH20 type, and adopt electrochemical principle to detect, resolution is 0.01ppm.Pump suction type formaldehyde air detection instrument makes pressurized capsule air flow, and has broken textile surface concentration of formaldehyde balance, has accelerated Form aldehyde release speed.
Below by experimental verification the inventive method.
1. sample preparation
Preparation 75mg/L, 150mg/L, 375mg/L tri-kinds of variable concentrations formalin, then the textile white tee shirt shirt without any process is immersed in the formalin of above-mentioned variable concentrations respectively, under being placed in room temperature condition, lucifuge soaks 3h, take out sample afterwards and squeeze unnecessary formalin gently, put into constant temperature oven respectively, tile drying 1h under 50 DEG C of conditions.Sample Polythene Bag after oven dry seals respectively and holds, and outer aluminium foil is In Shade saves backup.The T-shirt that immersion concentration of formaldehyde is respectively 75mg/L, 150mg/L, 375mg/L is labeled as sample A, sample B, sample C successively.Due to formaldehyde highly volatile, for preventing that formaldehyde transfer occurs between different sample, each sample makes separately and seals preservation.
2. content of formaldehyde test
(1) testing sample is put into pressurized capsule, then pressurized capsule is put into constant temperature oven, by rubber hose, the air intake opening of pump suction type formaldehyde air detection instrument and gas outlet are passed into pressurized capsule inside respectively.
(2) set the experimental temperature of constant temperature oven, rise to experimental temperature and after constant temperature certain hour, the formaldehyde contained in sample just can be released slowly into sealing cabin inside until temperature.
(3) directly read the content of formaldehyde in pressurized capsule in air after being with pump suction type formaldehyde air detection instrument stable reading, the gas after detection is got back in sealing cabin through the gas outlet of pump suction type formaldehyde air detection instrument.
(4) clean pressurized capsule with distilled water after off-test, avoid removing residue formaldehyde to affect next experimental result.
3. interpretation
3.1 experiment of single factor and Orthogonal experiment results
(1) time is on the impact of test result
When other experiment conditions are constant, sample A is put into pressurized capsule, heat under 50 DEG C of constant temperatures, record the display data of detector at interval of certain hour, experimental result is shown in Fig. 1.
As shown in Figure 1, when other test condition is constant, the formaldehyde that the increase textile along with experimental period discharges increases gradually, and after certain hour, concentration of formaldehyde is stable gradually no longer increases.By the curvilinear equation Y=-1.2351+3.92443X-0.24755x of matching
2, during heated at constant temperature 7.9h known by equation, in pressurized capsule, concentration of formaldehyde reaches maximal value.At 0 ~ 4h Form aldehyde release initial stage, the concentration of formaldehyde of textile surface is higher, and evaporation rate is very fast; Along with the prolongation of release time, the concentration of formaldehyde that textile shows reduces gradually, and the release rate of formaldehyde slows down, after this stage occurs in 4 ~ 6h; Concentration of formaldehyde after 6h in textile and the concentration of formaldehyde in air reach balance gradually, and the concentration of formaldehyde in pressurized capsule tends towards stability; In 8 ~ 10h pressurized capsule, concentration of formaldehyde reaches maximal value and keeps constant.
(2) temperature is on the impact of test result
Choose sample A as sample, sample is put into pressurized capsule, respectively temperature is set to 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C and constant temperature maintenance.In process of the test, the data under 2 hour records, detector shown, so that the Form aldehyde release speed of observing.Fig. 2 is the release conditions of formaldehyde at different time, temperature.
As shown in Figure 2, the release of temperature PARA FORMALDEHYDE PRILLS(91,95) plays a part key, and higher temperature can not only impel Form aldehyde release can also improve the release rate of formaldehyde.During heated at constant temperature 4h, the burst size of 30 DEG C of formaldehyde is only 2.36ppm, and the concentration of formaldehyde in 60 DEG C of environment has reached 13.37ppm, can find thus, and high temperature can accelerate the release rate of formaldehyde, impels formaldehyde to discharge as early as possible.But higher temperature can cause certain damage to textile.Synthesise various factor considers that we select 50 DEG C as test temperature.
(3) sample content of formaldehyde is on the impact of test result
The how many impact on testing result of sample content of formaldehyde can not be ignored, the sample that we choose three kinds of content of formaldehyde different to this detects it under identical experiment condition, temperature is set as 50 DEG C, the time is 8h, detects the content of formaldehyde of sample A, sample B and sample C respectively.Experimental result is shown in Fig. 3.
As shown in Figure 3, the formaldehyde emission quantities of three kinds of samples is substantially identical, the sample that content of formaldehyde is higher, and test result is also larger.The release of formaldehyde in textile is generally divided into three phases: the initial stage be discharge the stage fast, be then the slow releasing stage, finally reach stable equilibrium.
(4) orthogonal test
Investigate influence factor and optimal level in experiment by orthogonal test, show with time, temperature and sample for factor design Three factors-levels orthogonal test, factor level is in table 1.
Table 1 quadrature factor table
Table 2 Orthogonal experiment results
As shown in Table 2, the impact order of influence factor on experimental result of formaldehyde content of textiles pressurized capsule detection method is followed successively by sample > time > temperature, because the impact of sample mainly refers to the impact that in sample, concentration is how many, therefore the impact of sample is removed, considering optimum experiment condition is A3 and temperature 60 C, B2 and time 8h, because the higher meeting of temperature causes damage to textile, temperature is set as 50 DEG C by us.
3.2 with the contrast of national standard test result
Due to the difference of method of testing and experiment condition, test process and result also have larger difference.In order to observe the similarities and differences between different method of testing, the aqueous extraction method using standard GB/T/T2912.1-2009 " the mensuration part 1 of textile formaldehyde: the formaldehyde (aqueous extraction method) of free and hydrolysis " and GB/T2912.2-2009 " the mensuration part 1 of textile formaldehyde: the formaldehyde (vapor adsorption method) of release " to specify respectively, vapor absorption method and the content of formaldehyde detected in pressurized capsule detection method measurement sample A, sample B and sample C, the most at last test result mapping analysis observe its correlativity.Table 3 is the test findings of different detection method.
The different method of testing test result of table 3
Fig. 4 and Fig. 5 is the linear fit curve that the content of formaldehyde of pressurized capsule method of testing and national standard detect the testing result of aqueous extraction method and vapor absorption method.From Fig. 4 and Fig. 5, the testing result that the content of formaldehyde of pressurized capsule detection method test of the present invention and national standard detect vapor absorption method and aqueous extraction method has linear relationship.The linear correlation equation that pressurized capsule detection method and national standard detect aqueous extraction method is y=2.98741x-6.50991, and related coefficient is 0.98989; The linear correlation equation that pressurized capsule detection method and national standard detect vapor absorption method is y=3.10375x+11.03532, and related coefficient is 0.9895.
Analyzed known by the above results, the testing result of pressurized capsule detection method is low compared with the testing result of national standard detection method, but the content of formaldehyde that pressurized capsule detection method detects and the experimental result that national standard method detects have good linear relationship, have good correlativity.Therefore, can be similar to according to linear equation relation pressurized capsule detection method testing result the testing result replacing national standard.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change above-mentioned embodiment and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this instructions, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (3)
1. a formaldehyde content of textiles pressurized capsule method of testing, is characterized in that, the method adopts following step:
1) sample is put into pressurized capsule, then pressurized capsule is put into constant temperature oven, by rubber hose, the air intake opening of pump suction type formaldehyde air detection instrument and gas outlet are linked into pressurized capsule inside respectively;
2) temperature 50 C of constant temperature oven is set, treats that temperature rises to 50 DEG C and heated at constant temperature 8h ~ 10h; In this process, the formaldehyde contained in sample just can be released slowly into pressurized capsule inside, and inner for the pressurized capsule gas with formaldehyde flows back and forth by pump suction type formaldehyde air detection instrument between its detection place and pressurized capsule;
3) observe the reading of pump suction type formaldehyde air detection instrument, after stable reading, directly read formaldehyde content values and record, detecting and namely come to an end;
4) by 3) in the formaldehyde content values that reads be converted into the weight content value of sample, namely the data value in units of mg/Kg, and substituted in formula y=2.98741x-6.50991 or y=3.10375x+11.03532 and calculate, show that the value of y is the final formaldehyde content values of sample.
2. formaldehyde content of textiles pressurized capsule method of testing according to claim 1, it is characterized in that, the method adopts following equipment:
Comprise pressurized capsule, constant temperature oven and pump suction type formaldehyde air detection instrument, described pressurized capsule is complete seal cavity, only stays two small through hole for connecting pump suction type formaldehyde air detection instrument; Described two small through hole are positioned at the not coplanar of pressurized capsule or the both sides of the same face; The air intake opening of described pump suction type formaldehyde air detection instrument is connected with two small through hole of pressurized capsule by rubber hose respectively with gas outlet, forms steam circuit; Described constant temperature oven is transformed on commercially available a conventional oven, and design increase by two small sized pipelines can for inserting rubber hose.
3. formaldehyde content of textiles pressurized capsule method of testing according to claim 2, is characterized in that, described pump suction type formaldehyde air detection instrument is commercially available POT400-CH20 type, and adopt electrochemical principle to detect, resolution is 0.01ppm.
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| CN105510476A (en) * | 2015-12-30 | 2016-04-20 | 田琳琳 | Method for measuring formaldehyde in textile |
| CN107843547A (en) * | 2017-12-22 | 2018-03-27 | 鲁丰织染有限公司 | The method for detecting textile formaldehyde aging |
| CN110514694A (en) * | 2019-09-26 | 2019-11-29 | 王公华 | Textile material thermal insulation property test method and tester based on ambient temperature compensation |
| CN113341110A (en) * | 2021-07-09 | 2021-09-03 | 天津工业大学 | Method for detecting fragrance lasting property of aromatic textile |
| CN113655180A (en) * | 2021-08-23 | 2021-11-16 | 安徽省汉博科技有限公司 | High-precision furniture formaldehyde detection device and method |
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| CN113655180A (en) * | 2021-08-23 | 2021-11-16 | 安徽省汉博科技有限公司 | High-precision furniture formaldehyde detection device and method |
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Application publication date: 20151223 |