CN102998379A - Method for detecting contents of benzene, methylbenzene and ethylbenzene in high-purity ammonia - Google Patents
Method for detecting contents of benzene, methylbenzene and ethylbenzene in high-purity ammonia Download PDFInfo
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Abstract
The invention discloses a method for detecting the contents of benzene, methylbenzene and ethylbenzene in high-purity ammonia, wherein the reaction mechanism is as follows: the method comprises the following steps of: charging high-purity ammonia gas in a 100 mL clean volumetric flask filled with 50 mL of diisopropanolamine solution, and calculating the weight of the ammonia gas by virtue of a difference method; then heating the ammonia gas in a water bath at 60 DEG C, volatilizing the ammonia gas by virtue of the characteristic that the substances such as benzene, methylbenzene and ethylbenzene are extremely easy to dissolve in the diisopropanolamine solution, quantitatively detecting the contents of benzene, methylbenzene and ethylbenzene by virtue of an internal standard method, and finally calculating the contents of benzene, methylbenzene and ethylbenzene in the ammonia gas. The method disclosed by the invention is used for detecting the contents of benzene, methylbenzene and ethylbenzene in the high-purity ammonia, and has the advantages of being simple to sample, simple and convenient to operate, low in cost, fast in analysis speed, high in detection accuracy, low in detection limit and short in analysis cycle.
Description
Technical field
The present invention relates to the detection method of impurity in a kind of gas, particularly a kind of method that detects benzene in the high-purity ammon, toluene and ethylbenzene content.
Background technology
4.5N high-purity ammon is a kind of very important raw material in the food additives, in our daily life, closely related with us, almost ubiquitous, so to say that, if do not have food additives that color, form and the quality etc. of food just can not be arranged, just do not have our today of colourful life yet.And ammonium glycyrrhetate is to touch the most general food additives in our daily life: the glycyrrhizic acid powder is dissolved in the organic solvent solution refluxing extraction, adds ammonia or ammoniacal liquor, filtration, drying namely get ammonium glycyrrhetate; Ammonium glycyrrhetate has anti-hepatotoxicity, is by an active component that extracts in the glycyrrhiza uralensis fisch, reduces glutamic-pyruvic transaminase, recovers hepatocyte function, prevents the effects such as Steatosis; Promote BILE PIGMENTS metabolism and removing jaundice and detoxication, reduce the collagenous fibres hyperplasia, prevent cirrhosis etc.The sugariness of its principal ingredient is 200-300 times of sucrose, aspect food additives, have low calorie, safety non-toxic and stronger medicinal health care function, it is the most desirable sweetener of hypertension, obesity, diabetes, cardiac's use, strong Radix Glycyrrhizae peat-reek is arranged, having health care, detoxify, protect the effects such as liver, anti-inflammatory, flavouring, is ideal pure natural sweetener raw material; Be applied in canned meat, flavoring, flavouring, soy sauce, beans sauce, salad dressing, curing food, frozen confectionery, chewing gum, betel nut, bread food, sweetmeat, biscuit, low-carbohydrate food, sugarfree foods, fruit juice, dairy products, milk powder, functional beverage etc. mainly as food additives.
And the second largest food additives in our daily life are quaternary ammonium salts, are raw material with fatty acid, make Arneel SD through ammonification, are fatty amine through hydrogenation again, then with primary amine and bromoalkane reaction, namely get quaternary ammonium salt.The breeding of bacterium algae and the generation of foundry loam in can establishment food, thus play sterilization, press down mould and mothproof function; Simultaneously polyquaternium also have certain deoil, the use of deodorizing and slowly-releasing, played the food fresh keeping effect; Main canned meat that germifuge and antiseptic be widely used in the supermarket, soy sauce, beans sauce, salad dressing, curing food, frozen confectionery, bread food, sweetmeat, low-carbohydrate food, sugarfree foods, fruit juice, meat product etc. of being used as.
If contain benzene, toluene and ethylbenzene in the food, the words health effects that is absorbed by the body is very fearful.Be mainly manifested in: they mainly have superpower destruction to eye, respiratory tract, skin and blood etc.Benzene is summed up as 3 kinds to the harm of health: carcinogenic, disable, the teratogenesis tire; Take in benzene in short time acute benzene toxicity can occur, excitement or feeling groggy occur, with the mucosa irritation symptom.Gently then dizzy, headache, feel sick, vomiting, instability of gait; Heavy then go into a coma, tic and circulatory failure be until death; Subacute benzene poisoning can occur in the long-term benzene of taking in, and the symptoms such as giddy, headache, weak, insomnia, paramenia occur, and alpastic anemia, acute leukemia can occur, and shows as the anaemia that develops rapidly, hemorrhage, infection etc.Benzene has inhibiting effect to the hematopoiesis function of human body, can make red blood cell, leucocyte and decrease of platelet.Benzene works the mischief to hemopoietic system simultaneously, can cause the systemic diseases such as anaemia, infection, subcutaneous hemorrhage.
Can make people's brain and kidney be subject to permanent damage after taking in toluene; Can injure hearing for a long time, cause the problems such as headache, dizzy, weak, pale, hypopsia and equilibrium function imbalance; Blurred vision can appear in severe intoxication, trembles, breathes shallow and fast, chamber property heart murmur, tic, delirium and stupor.The serious case of minority can occur breathing and circulatory failure ventricular fibrillation.Take at period of gestation such as mother, its murder by poisoning can affect the baby and produce birth defects etc.
Can have than strong and stimulating skin, mucous membrane after taking in ethylbenzene, high concentration has anesthetic action: calomel poisoning has dizziness, headache, feels sick, vomits, lurchs, the slight disturbance of consciousness and eye and upper respiratory tract irritation; Severe one is gone into a coma, tic, blood pressure drops and respiratory and circulatory failure, neurasthenic syndrome; Liver there is certain infringement; Also can cause chemical pneumonia and pulmonary edema etc.
Therefore, 4.5N being food additives, high-purity ammon makes the crucial supplementary material in important upstream, field, control to its benzene, toluene and ethylbenzene is one of developing key link of industrial chain, is directly determining the development of food service industry, has been subject to people's energetically concern and attention at present.But at home in the additives industries prior art, in the standard about ammonia, all not mentioned monitoring and detections to benzene, toluene and ethylbenzene.And the benzene in the high-purity ammon, toluene and ethylbenzene are mainly derived from raw material ammonia: hydrogen is as one of raw material of synthesis material ammonia, and hydrogen produces by natural gas pyrolysis, all is not well controlled in cracking and synthetic process like this; In general, its benzene class content is all lower, all is to be the large molecular forms of gaseous state or gaseous state to exist, and does not have at present special method to detect, and can only vaporize or adsorbs or the method such as dissolving by suitable mode, and then utilize checkout equipment to carry out quantitatively; Simultaneously, ammonia is a kind of mordant gas, numerous technician are headache for it, all seek a kind of direct gas sampling method always and detect benzene, toluene and ethylbenzene in the ammonia, but direct injected can the burn into damage even damaged chromatogram and chromatographic column.Although direct injected is easier, brought significantly burn into damage even breaking-up chromatographic apparatus for simultaneously chromatograph and chromatographic column; Because the material of chromatograph and chromatographic column all is stainless steel, and ammonia very easily corrodes the stainless steel material at normal temperatures, instrument is caused fatefulue breaking-up.The instrument of completely newly devoting oneself to work, general three wheat harvesting periods just need to change chromatographic column and consumptive material, even just allow instrument work in a few week, repair all to want more than 20,000 yuan general at every turn, and wasted a large amount of time, so seriously hindered our routine testing.
Summary of the invention
Goal of the invention of the present invention is in order to overcome the shortcoming of above-mentioned background technology, and the method for benzene, toluene and ethylbenzene content in a kind of detection high-purity ammon effective and that come by the indirect sample introduction mode is provided.
The technical scheme of patent of the present invention is: a kind of method that detects benzene in the high-purity ammon, toluene and ethylbenzene content is characterized in that this method realizes by following processing step:
(1) preparation of sample solution: directly high-purity ammon is passed in the volumetric flask of 50mL diisopropanol amine aqueous solution and dissolve, after the certain hour, by front and back the of poor quality for passing into the quality of ammonia of volumetric flask of weighing; At last the above-mentioned sample of producing is put into 60 ℃ heating water bath 50～60 minutes, then be cooled to the room temperature in laboratory;
(2) preliminary work of instrument: pass into first helium, the flow that its carrier gas is set is 30mL/min, then starts instrument; Open air and hydrogen when temperature rises to 100 ℃, the flow of air is 400mL/min, and the flow of hydrogen is 35mL/min, lights chromatographic hydrogen flame detector FID, and the flow set of hydrogen is 45mL/min during igniting, waits for the steadily rear sample introduction of baseline;
(3) drafting of typical curve: add the diisopropanol amine aqueous solution of 200mL to the volumetric flask of the 1000mL of cleaning, more respectively accurately benzene, toluene and the ethylbenzene solution of weighing 0.5 gram splash into this volumetric flask, be accurate to 0.0001 gram; Then use the diisopropanolamine solution dilution to the scale mark 1000mL of volumetric flask, mother liquor about 500ppm completes; Then in the volumetric flask of the diisopropanolamine that fills 50mL, pipette respectively 0.1mL with transfer pipet, 0.2mL, 0.5mL, 2mL, the above-mentioned 500ppm mother liquor of 5mL and 5mL is also accurately weighed, and is accurate to 0.0001 gram; Adding the 10uL sec-butyl alcohol in the most backward each bottle is target content in interior mark and the accurate weighing, then is settled to the 50mL scale mark with the diisopropanol amine aqueous solution, is configured to 1ppm, 2ppm, 5ppm, 10ppm, these six kinds of specification standards solution of 20ppm and 100ppm; The 2mL auto injection bottle of packing into is at last done the reagent blank of a 2mL diisopropanolamine simultaneously, and sortord is that blank is placed above the other things, other solution bottles by concentration from low to high, are placed in the automatic sampler successively, allow its auto injection, simultaneously tail piping and druming is opened, the flow that tail blows is 5mL/min;
(4) area that at last peak area of each standard specimen deduction reagent blank is obtained is the area of standard specimen, do the typical curve that interior mark is produced a content and area with sec-butyl alcohol simultaneously, check that the regression coefficient of typical curve can accept more than 99%, otherwise sample introduction, data are processed again, can until satisfy condition;
(5) detecting step
(a) add the 10uL sec-butyl alcohol in the ready sample solution and do interior mark, accurate target quality in weighing and the record is put into the program that has editted and is allowed the automatic sampler auto injection; At least prepare two groups of samples, each sample feeding number of times is at least 3 times, asks at last the mean value of sample; Gap can be accepted within 3% between the area of same sample and the mean value, and the area difference distance between the different samples can be accepted within 5%, otherwise reconfigures sample, can until condition is satisfied;
(b) call at last the working curve of above-mentioned steps (2), directly calculate benzene, toluene and ethylbenzene content in the diisopropanol amine aqueous solution; Last again by calculating benzene, toluene and the ethylbenzene content in the ammonia;
(c) at last the furnace temperature of instrument is risen to 300 ℃ of aging pillars, simultaneously tail is blown and be set to 20 mL/min, ammonia residual in the diethanolamine and some high-boiling components etc. is driven out of, otherwise can pollute pillar and affect the testing result of next time, even can corrode the accessory of gas chromatography; Simultaneously the access of the other end of tail gas is contained in the 5% dilute hydrochloric acid solution slot container, fully absorb ammonia and prevent from discharging and the air pollution that causes etc.;
(d) 300 ℃ of aging pillars were cooled to 40 ℃ and just close chromatograph after 2～3 hours, closed at last source of the gas.
The invention has the beneficial effects as follows: this indirect sample introduction method of the present invention has solved the etching problem to equipment: utilize benzene, toluene and ethylbenzene in the ammonia very easily to dissolve in diisopropanol amine aqueous solution and highly stable solution, heat a little again the ammonia that will dissolve in the diisopropanol amine aqueous solution and evaporate, last benzene, toluene and the ethylbenzene content of dissolving in the diisopropanol amine aqueous solution that detect again.Like this; the diisopropanol amine aqueous solution approaches neutral; sampling system and detection system etc. all there is not corrosivity; simultaneously replace packed column with capillary column again; be isolated effect and increased by 10 ~ 15 times; simultaneously the detectability of instrument is brought up to 0.05ppm; later on high-boiling components was blown with certain tail in 2 ~ 3 hours by 300 ℃ of aging pillars more at last and bring out; allow daily testing not polluted by the detection of sample last time and obtained guarantee; protected well simultaneously instrument; for supervisory function bit has been played in production and the internal control of high-purity ammon, technical support and guarantee are provided for rationalizing to produce simultaneously.It is simple that the present invention also has sampling, and easy and simple to handle, with low cost, analysis speed is fast, the advantage that accuracy of detection is high.
Embodiment
Fig. 1 is the content of benzene and the typical curve of area;
Fig. 2 is the content of toluene and the typical curve of area;
Fig. 3 is the content of ethylbenzene and the typical curve of area.
1. reagent and gas
(1) sec-butyl alcohol: have another name called the 2-butanols, it is pure to require to be at least analysis;
(2) benzene, toluene and ethylbenzene: purity is at least 99.9%;
(3) helium, hydrogen and nitrogen: purity is at least 99.999%;
2. instrument and equipment
(1) GC6890 chromatograph: Agilent science and technology (China) company limited (hydrogen flame detector FID);
(2) HP-1 capillary chromatographic column: long 25m, internal diameter 0.32mm, thickness 0.52um;
(3) electronic balance: can be accurate to 0.0001 gram;
(4) GC6890 automatic sampler: buy to Agilent company, have at least 10 sample feeding dishes are arranged;
(5) auto injection bottle: buy to Agilent company, specification is 2.0mL, is furnished with sample pad and sample lid;
(6) volumetric flask: 100mL;
(7) water-bath: be at least two holes;
3. chromatographic condition
Injector: 250 ℃; Detecting device: 250 ℃;
Temperature programme: furnace temperature kept 5 minutes since 50 ℃, was warming up to 150 ℃ with 10 ℃/min afterwards and kept 5 minutes again, rose to 250 ℃ with 20 ℃/min at last and kept 10 minutes;
Column flow rate: 1.0mL/min, split ratio is 50:1, the auto injection volume is 1.0uL.
4. the preparation of sample
(1) each sample is according to following disposal route: get clean 100mL tool plug volumetric flask, add 50mL diisopropanol amine aqueous solution and build simultaneously lid, then be placed on and take by weighing weight on the electronic balance, be accurate to 0.0001g, record weight is m
1The teflon hose that to take one section diameter be 0.125cm, the one end is connected on the high-purity ammon storage tank with special jointing, the other end of flexible pipe directly inserts in this volumetric flask, open storage tank valve, directly high-purity, ultra-pure ammonia are passed in the water and dissolve, flow is the 200-220mL per minute, take a sample and stop after 50-60 minute, after treating that one section no liquid of this tetrafluoroethene flexible pipe flows out, take out this pipe and cover lid at the uniform velocity, the weight of record this moment is m
2, calculate the high-purity weight that is dissolved in the diisopropanolamine, i.e. m=m with difference assay
2-m
1
Attention: the thickness of plastic flexible pipe is to connect rear air tight being advisable, ammonia is passed into relevant device must clean totally in the capacity, will pass into ammonia to be measured before sampling purges several times, and can not have liquid to spill volumetric flask in the experimentation, the flow that passes into ammonia is as the criterion with the bubble of not emerging outside liquid level.
(2) the above-mentioned sample of producing is put into 60 ℃ heating water bath 50 ~ 60 minutes, then be cooled to laboratory temperature, be settled to scale mark with diisopropanolamine again, this is sample solution;
(3) this sample solution is prepared two groups at least, calculates its average content.
5. preliminary work
(1) pass into first helium, the flow that its carrier gas is set is 30mL/min, then starts instrument; Open air and hydrogen when temperature rises to 100 ℃, the flow of air is 400mL/min, and the flow of hydrogen is 35mL/min, and when lighting the FID(igniting, the flow of hydrogen is that the flow of hydrogen is 45mL/min); According to above-mentioned steps 3 instrument is set; Until the steadily rear sample introduction of baseline, in the time of sample introduction tail piping and druming to be opened, the flow that tail blows is 5mL/min;
(2) add benzene, toluene and ethylbenzene solution through accurate weighing in the volumetric flask of the diisopropanolamine that fills 50mL, simultaneously adding the 10uL sec-butyl alcohol in each bottle is target content in interior mark and the accurate recording, be settled to scale mark with diisopropanolamine at last, be configured to 1ppm, 2ppm, 5ppm, 10ppm, these six kinds of specification standards solution of 20ppm and 100ppm;
(3) add diisopropanolamine reagent in the auto injection bottle and do blank, (place in order by blank for 6 kinds of standard solution that will configure again, other solution are according to concentration from low to high) arrange and be placed on the automatic sampler, automatic sampler is set by its auto injection according to above-mentioned steps 3, each sample repeats the mean value of sample introduction 5 times and reference area at least, the area of every component and mean value difference can be accepted with interior 5%, otherwise sample introduction again, until till condition satisfies;
(4) utilize the boiling point of each component different, the collection of illustrative plates that separates in chromatographic column sequentially is benzene, toluene and ethylbenzene; At last with the area of the Area subtraction blank of each component, the content of remaining area and itself and component is produced the typical curve of a content and area (such as table 1-3, Fig. 1-3), then check that the regression coefficient of typical curve can accept more than 99.5%, otherwise sample introduction, data are processed again, can until satisfy condition;
The correspondence table of the content of table 1. benzene--area
The corresponding table of table 2. toluene level and area
| Content (ppm) | 0.95 | 1.9 | 4.9 | 9.5 | 19．1 | 95.1 |
| Area (pA.s) | 2.689 | 5.341 | 11.777 | 28.414 | 52.586 | 228.737 |
The corresponding table of table 3. ethylbenzene benzene content and area
| Content (ppm) | 1.0 | 2.0 | 5.0 | 10.0 | 20.0 | 100.0 |
| Area (pA.s) | 2.689 | 5.341 | 11.777 | 28.414 | 52.586 | 228.737 |
(5) can find that by experiment there are certain ratio in the content of every kind of material and area, and this ratio we be referred to as improvement factor RF, the concentration of the content of this material of RF=/this material;
(6) at last this standard working curve is filed and name, quick and precisely use in the time of for test sample;
Remarks: the inferior typical curve cycle is a week, preferably again makes working curve before each the detection; Use standard specimen with the sample related concentrations standard specimen that tries again to reclaim after perhaps detecting, the standard specimen recovery can be accepted between 95%-105%, otherwise need to again make working curve;
6. detecting step
(1) adding the 10uL sec-butyl alcohol in the sample solution of producing according to above-mentioned steps 4 is target content in interior mark and the accurate recording;
(2) then sample solution is placed on automatic sampler, its auto injection of band instrument stabilizer relief, the number of times of sample introduction is at least 3 times, asks at last the mean value of sample solution; Gap can be accepted within 3% between the area of same sample and the mean value, and the gap between the different samples can be accepted within 5%, otherwise reconfigures sample, can until condition is satisfied;
(3) the last above-mentioned standard working curve of bar directly reads each component concentration of sample;
(4) at last the furnace temperature of instrument is risen to 300 ℃ of aging pillars, tail is blown be set to 20 mL/min simultaneously, ammonia residual in the diethanolamine is driven out of, otherwise can pollute pillar and affect the testing result of next time, even can corrode the accessory of gas chromatography; Simultaneously the access of the other end of tail gas is contained in the 5% dilute hydrochloric acid solution slot container, fully absorb ammonia and prevent from discharging and the air pollution that causes etc.;
Remarks: each testing is finished, waste liquid is poured in the waste liquid barrel, simultaneously with this slot container with cleaning up and drying, in order to use next time;
(5) 300 ℃ of aging pillars were cooled to 40 ℃ and just close chromatograph after 2 ~ 3 hours, closed at last source of the gas.
7. calculate
Just can calculate the content (c) of benzene in the diisopropanol amine aqueous solution, toluene and each component of ethylbenzene according to instrument formula (1).
The content (ppm) of c-this component in the diisopropanol amine aqueous solution wherein;
The peak area (pA.s) of A-this component in the diisopropanol amine aqueous solution;
RF-the correction factor of this component in the diisopropanol amine aqueous solution;
The content (ppm) of mark sec-butyl alcohol in Ci-this diisopropanol amine aqueous solution
The peak area (pA.s) of mark sec-butyl alcohol in Ai-this diisopropanol amine aqueous solution
The content of the benzene in high-purity ammonia, toluene and every kind of component of ethylbenzene calculates respectively according to following formula (2):
The content (ppm) of t-this component in ammonia wherein;
The content (ppm) of c-this component in the diisopropanol amine aqueous solution;
D-above-mentioned diisopropanolamine liquid density (g/mL);
The quality of m-ammonia (g).
Claims (4)
1. method that detects benzene in the high-purity ammon, toluene and ethylbenzene content is characterized in that this method realizes by following processing step:
(1) preparation of sample solution: directly high-purity ammon is passed in the volumetric flask of 50mL diisopropanol amine aqueous solution and dissolve, after the certain hour, by front and back the of poor quality for passing into the quality of ammonia of volumetric flask of weighing; At last the above-mentioned sample of producing is put into 60 ℃ heating water bath 50～60 minutes, then be cooled to the room temperature in laboratory;
(2) preliminary work of instrument: pass into first helium, the flow that its carrier gas is set is 30mL/min, then starts instrument; Open air and hydrogen when temperature rises to 100 ℃, the flow of air is 400mL/min, and the flow of hydrogen is 35mL/min, lights chromatographic hydrogen flame detector FID, and the flow set of hydrogen is 45mL/min during igniting, waits for the steadily rear sample introduction of baseline;
(3) drafting of typical curve: add the diisopropanol amine aqueous solution of 200mL to the volumetric flask of the 1000mL of cleaning, more respectively accurately benzene, toluene and the ethylbenzene solution of weighing 0.5 gram splash into this volumetric flask, be accurate to 0.0001 gram; Then use the diisopropanolamine solution dilution to the scale mark 1000mL of volumetric flask, mother liquor about 500ppm completes; Then in the volumetric flask of the diisopropanolamine that fills 50mL, pipette respectively 0.1mL with transfer pipet, 0.2mL, 0.5mL, 2mL, the above-mentioned 500ppm mother liquor of 5mL and 5mL is also accurately weighed, and is accurate to 0.0001 gram; Adding the 10uL sec-butyl alcohol in the most backward each bottle is target content in interior mark and the accurate weighing, then is settled to the 50mL scale mark with the diisopropanol amine aqueous solution, is configured to 1ppm, 2ppm, 5ppm, 10ppm, these six kinds of specification standards solution of 20ppm and 100ppm; The 2mL auto injection bottle of packing into is at last done the reagent blank of a 2mL diisopropanolamine simultaneously, and sortord is that blank is placed above the other things, other solution bottles by concentration from low to high, are placed in the automatic sampler successively, allow its auto injection, simultaneously tail piping and druming is opened, the flow that tail blows is 5mL/min;
(4) area that at last peak area of each standard specimen deduction reagent blank is obtained is the area of standard specimen, do the typical curve that interior mark is produced a content and area with sec-butyl alcohol simultaneously, check that the regression coefficient of typical curve can accept more than 99%, otherwise sample introduction, data are processed again, can until satisfy condition;
(5) detecting step
(a) add the 10uL sec-butyl alcohol in the ready sample solution and do interior mark, accurate target quality in weighing and the record is put into the program that has editted and is allowed the automatic sampler auto injection; At least prepare two groups of samples, each sample feeding number of times is at least 3 times, asks at last the mean value of sample; Gap can be accepted within 3% between the area of same sample and the mean value, and the area difference distance between the different samples can be accepted within 5%, otherwise reconfigures sample, can until condition is satisfied;
(b) call at last the working curve of above-mentioned steps (2), directly calculate benzene, toluene and ethylbenzene content in the diisopropanol amine aqueous solution; Last again by calculating benzene, toluene and the ethylbenzene content in the ammonia;
(c) at last the furnace temperature of instrument is risen to 300 ℃ of aging pillars, simultaneously tail is blown and be set to 20 mL/min, ammonia residual in the diethanolamine and some high-boiling components etc. is driven out of, otherwise can pollute pillar and affect the testing result of next time, even can corrode the accessory of gas chromatography; Simultaneously the access of the other end of tail gas is contained in the 5% dilute hydrochloric acid solution slot container, fully absorb ammonia and prevent from discharging and the air pollution that causes etc.;
(d) 300 ℃ of aging pillars were cooled to 40 ℃ and just close chromatograph after 2～3 hours, closed at last source of the gas.
2. the method for benzene, toluene and ethylbenzene content in the detection high-purity ammon as claimed in claim 1, it is characterized in that the ammonia quality in the above-mentioned steps (1) calculates by the following method: get clean 100mL tool plug volumetric flask, add 50mL diisopropanol amine aqueous solution and build simultaneously lid, then be placed on and take by weighing weight on the electronic balance, electronic balance is accurate to 0.0001g, and record weight is m
1The teflon hose that to take one section diameter be 0.125cm, the one end is connected on the high-purity ammon storage tank with special jointing, the other end of flexible pipe directly inserts in this volumetric flask, open storage tank valve, directly high-purity, ultra-pure ammonia are passed in the water and dissolve, flow is 200～220mL per minute, take a sample and stop after 50～60 minutes, after treating that one section no liquid of this tetrafluoroethene flexible pipe flows out, take out this pipe and cover lid at the uniform velocity, the weight of record this moment is m
2, calculate the high-purity weight that is dissolved in the diisopropanolamine, i.e. m=m with difference assay
2-m
1
3. the method for benzene, toluene and ethylbenzene content in the detection high-purity ammon as claimed in claim 1 is characterized in that by following parameter chromatograph being set: injector: 250 ℃; Detecting device: 250 ℃; Temperature programme: furnace temperature kept 5 minutes since 50 ℃, was warming up to 150 ℃ with 10 ℃/min afterwards and kept 5 minutes again, rose to 250 ℃ with 20 ℃/min at last and kept 10 minutes; Column flow rate: 1.0mL/min, split ratio is 50:1, the auto injection volume is 1.0uL.
4. the method for benzene, toluene and ethylbenzene content in the detection high-purity ammon as claimed in claim 1 is characterized in that the content of benzene, toluene and each composition of ethylbenzene in the diisopropanol amine aqueous solution during described step (5) is (b) is by obtaining that following formula (1) calculates respectively:
The content (ppm) of c-this component in the diisopropanol amine aqueous solution wherein;
The peak area (pA.s) of A-this component in the diisopropanol amine aqueous solution;
RF-the correction factor of this component in the diisopropanol amine aqueous solution;
The content (ppm) of mark sec-butyl alcohol in Ci-this diisopropanol amine aqueous solution;
The peak area (pA.s) of mark sec-butyl alcohol in Ai-this diisopropanol amine aqueous solution;
The content of the benzene in high-purity ammonia, toluene and every kind of component of ethylbenzene calculates respectively according to following formula (2):
The content (ppm) of t-this component in ammonia wherein;
The content (ppm) of c-this component in the diisopropanol amine aqueous solution;
D-above-mentioned diisopropanolamine liquid density (g/mL);
The quality of m-ammonia (g).
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| CN104713961A (en) * | 2015-04-08 | 2015-06-17 | 神华集团有限责任公司 | Method for detecting ammonia component content in methyl alcohol |
| CN109580561A (en) * | 2018-10-17 | 2019-04-05 | 中国石油天然气集团有限公司 | A kind of three-dimensional fluorescence spectrum method of benzene homologues in measurement water |
| CN110546496A (en) * | 2017-04-25 | 2019-12-06 | 株式会社岛津制作所 | Sample analyzer |
| CN110988236A (en) * | 2019-12-03 | 2020-04-10 | 江苏恒信检验有限公司 | Method for detecting benzene, toluene and xylene in ethanol |
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| CN110988236A (en) * | 2019-12-03 | 2020-04-10 | 江苏恒信检验有限公司 | Method for detecting benzene, toluene and xylene in ethanol |
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