CN107907626A - A kind of method for measuring cable fire release total amount of halogen acid gas - Google Patents
A kind of method for measuring cable fire release total amount of halogen acid gas Download PDFInfo
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- CN107907626A CN107907626A CN201711115387.5A CN201711115387A CN107907626A CN 107907626 A CN107907626 A CN 107907626A CN 201711115387 A CN201711115387 A CN 201711115387A CN 107907626 A CN107907626 A CN 107907626A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention discloses a kind of method for measuring cable fire release total amount of halogen acid gas.Electric wire, cable are burnt in heating furnace, the halogen acid gas disengaged are fully absorbed with sodium hydroxide solution, make indicator with potassium chromate solution, with silver nitrate titration halogen ion X‑.Because halide is the salt of strong acid generation, generation AgX yellow-white precipitations are acted on silver nitrate first.After halide ion and silver ion whole chemical combination, excessive silver ion reacts generation pink precipitate with chromate ions, indicates titration end-point.Since the amount of the material of halogen ion is consumed AgNO3Material amount, thus calculate the amounts of the halogen acid gas disengaged.It is an advantage of the invention that：Titration end-point is obvious, easy to observe, so as to improve the accuracy of halogen acids assay.
Description
Technical field
The present invention relates to the determination techniques of evolved gas during fire-fighting burning, more particularly, to one kind measure cable fire release
The method of total amount of halogen acid gas.The assay method is that one kind is suitable for GB/T17650.1-1998《It is derived from cable or optical cable combustion
The test method part 1 of evolved gas during burning：The measure of hydracid total amount》, it is derived from gathering with halogenation for cable or cable configuration
The hydracid that mixture and halogen additive agent mixture based on compound are discharged in burning（Except hydrofluoric acid）Gas gross is surveyed
Fixed alternative.
Background technology
GB/T17650.1-1998《The test method part 1 of evolved gas when being derived from cable or optical cable burning：Hydracid is total
The measure of amount》Test method used in standard is that experiment material is heated in dry air stream, and the gas disengaged exists
Absorbed in 0.1M sodium hydroxide solutions, then measure the total amount of halogen acid gas.Specific method is：Make sodium hydroxide molten with nitric acid
Liquid is acidified and adds the 0.1M silver nitrate solutions of certain volume, using ammonium ferric sulfate as indicator, is dripped with 0.1M ammonium thiocyanates are counter
Determine surplus.The principle of this method is to work as NH4The same AgNO of SCN3After the reaction was complete, excessive SCN-Same NH4Fe(SO4)2Generation is red
Fe (SCN)6 3-Complex ion, so that directing terminal.But this method indicator discoloration is very unlikely to observe, terminal can not be accurate
Judge, be the main reason for causing to measure inaccuracy.
The content of the invention
In view of problem existing in the prior art, the present invention provides a kind of side for measuring cable fire release total amount of halogen acid gas
Method.
The present invention adopts the technical scheme that：A kind of method for measuring cable fire release total amount of halogen acid gas, it is measured
Step is as follows：
Step 1：Various experimental apparatus are cleaned up with distilled water；
Step 2：Surveyed sample of cable is precisely weighed, is subsequently placed in the combustion tube of tubular heating furnace and heats, then sample is burnt
The halogen acid gas of release are imported in the wash bottle equipped with sodium hydroxide solution and fully absorbed, and are measured with PH test paper；
Step 3：Solution in wash bottle is all moved into a certain amount of measuring bottles by connecting tube, and with distilled water flushing wash bottle,
The terminal of connecting tube and combustion tube, while flushing liquor is also poured into measuring bottle, then solution is appended in measuring bottle to one with distilled water
It is quantitative；
Step 4：Poured into a certain amount of solution in measuring cup taken amount bottle in beaker, then clean measuring cup 2-3 times with distilled water, will cleaned
The filtrate remained in measuring cup is poured into beaker, is fully shaken up；
Step 5：Into beaker plus 3~5 drip potassium chromates, make the solution in beaker in light yellow；
Step 6：Beaker is placed in the dropper of rack for test tube in the following, preparing titration；
Before titration, the silver nitrate solution drop bottle initial volume reading on rack for test tube is first recorded, is denoted as V1, open magnetic stirrer pair
Solution in beaker is stirred, appropriate to decontrol rack for test tube silver nitrate solution drop bottle cock, makes silver ion fully anti-with halogen ion
Should, form yellow-white precipitation；It is terminal that pink, which has just occurred, in the solution being persistently titrated in beaker, tightens silver nitrate solution drop bottle
Cock, records remaining silver nitrate solution volume reading in drop bottle at this time, is denoted as V2, you can calculate the nitric acid with halogen ion reaction
The volumetric usage V of silver：V=V2-V1, wherein V, V2、V1Unit：ml；The halogen acid gas amount of cable burning release is counted as follows
Calculate：
nHX = (V·10-3·MAg+)（VAlways/ VSample)/m
In formula：nHX：The halogen acid gas amount of cable burning release, unit：mol；
VSample：For the liquor capacity of drop reaction, unit：ml；
VAlways：Overall solution volume in measuring bottle, unit：ml；
MAg+：Silver nitrate solution molar concentration, unit：mol/L；
V：With the volume of the silver nitrate solution of halogen acid gas reaction, unit：ml；
m:The quality of cable, unit：g.
The present invention in step 2, will be precisely weighed 1g ± 0.1mg cable samples and be placed in the combustion tube of tubular heating furnace,
Then the halogen acid gas of sample burning release are imported in the wash bottle equipped with 200mL sodium hydroxide solutions and fully absorbed, then use PH
Test paper measures, it is desirable to which the pH value of solution is 7-8 at this time.
The molar concentration of sodium hydroxide solution of the present invention is 0.1 mol/L.
The present invention in step 3, then the sodium hydroxide solution in wash bottle is all moved into by connecting tube and a certain amount of is
In 1000mL measuring bottles, and with the terminal of distilled water flushing wash bottle, connecting tube and combustion tube, while flushing liquor is also poured into measuring bottle
In, it is 1000mL that it is a certain amount of, which to be then appended to solution in measuring bottle, with distilled water.
The present invention is 100ml with a certain amount of solution in measuring cup taken amount bottle in step 4.
In steps of 5, the concentration of potassium chromate is 5% to the present invention, i.e. 5g potassium chromates are dissolved in 95mL distilled water.
In step 6, silver nitrate solution molar concentration is 0.1 mol/L to the present invention.
It is an advantage of the invention that：Titration end-point is obvious, easy to observe, so as to improve the accurate of halogen acids assay
Degree.
The measuring principle of the present invention：Electricity（Line）Cable burns in heating furnace, the halogen acid gas sodium hydroxide solution disengaged
Fully absorb, with potassium chromate solution（K2CrO4）Make indicator, use silver nitrate（AgNO3）Titrate halogen ion X-（Cl-、Br-、I-）.
Because halide is the salt of strong acid generation, first with silver nitrate（AgNO3）Effect generation AgX yellow-white precipitations.Work as halide ion（X-）
And silver ion（Ag+）After whole chemical combination, excessive silver ion（Ag+）I.e. and chromate ions（CrO4 2-）Reaction generation pink is heavy
Form sediment, indicate titration end-point.Since the amount of the material of halogen ion is consumed AgNO3Material amount, thus calculate disengage
Hydracid（Except hydrofluoric acid）The amount of gas.
Reaction equation：
（1）The halogen acid gas of sample burning release are fully absorbed with sodium hydroxide solution first：
NaOH + HX → NaX + H2O (X Cl, Br, I)
（2）Drop reaction first stage, silver nitrate and halide reaction generation yellow-white precipitation：
NaX (halide)+AgNO3→ AgX ↓ (yellow-white precipitation)+NaNO3
（3）Drop reaction terminal point determining, excess nitrate and chromate ions are reacted into pink precipitate：
2AgNO3（It is excessive）+ K2CrO4 → 2KNO3 +Ag2CrO4↓ (pink precipitate).
Embodiment
The invention will be further described by the following examples；Embodiment.
First, using sample and reagent
1. 1g is electric（Line）Cable
2. distilled water
0.1M sodium hydroxides 3. (NaOH) solution（M is molar concentration）；
4. 0.1M silver nitrates (AgNO3) solution；
5. 5% potassium chromate (K2CrO4) solution（5g potassium chromates are dissolved in 95mL distilled water）；
6. PH test paper.
2nd, determination step
1st, various experimental apparatus are cleaned up with distilled water.
2nd, the electricity of 1g will be precisely weighed（Line）Cable sample is placed in the combustion tube of tube furnace, then in the hydracid of burning release
Gas is imported in the wash bottle of 0.1M sodium hydroxides (NaOH) solution equipped with 200mL and fully absorbed, and is measured with PH test paper,
It is 7-8 to seek sodium hydroxide solution PH.
0.1M sodium hydroxides (NaOH) solution of 200mL is through test of many times, can ensure to fully absorb the hydracid of generation
The dosage of gas, if special case PH test paper measure solution PH is less than 7, can increase NaOH solution dosage.
3rd, the solution in wash bottle is all moved into the measuring bottle of 1000mL by connecting tube again, and is washed with distilled water flushing
The terminal of bottle, connecting tube and combustion tube（After cooling）, while flushing liquor is also poured into measuring bottle, then with the distilled water amount of being appended to
Solution 1000mL in bottle.
4th, poured into the 100ml solution of solution in measuring cup taken amount bottle in 500ml beakers, then clean measuring cup 2 with distilled water
It is secondary, the filtrate that cleaning is remained in measuring cup is poured into beaker, is fully shaken up.
5th, toward in beaker plus 5% potassium chromate（K2CrO4）3~5 drops, make the solution in beaker in light yellow（It is not very bright
It is aobvious）.
6th, beaker is placed in the dropper of rack for test tube in the following, preparing to titrate；Before titration, the nitric acid of drop bottle on rack for test tube is first recorded
Silver（AgNO3）Liquor capacity reading, is denoted as V1, silver nitrate solution molar concentration is 0.1；Magnetic stirrer is opened in beaker
Solution is stirred, appropriate to decontrol rack for test tube silver nitrate solution drop bottle cock, makes silver ion（Ag+）With halogen ion (X-) fully anti-
Should, form yellow-white precipitation；It is terminal that pink, which has just occurred, in the solution being titrated in beaker, tightens the rotation of silver nitrate solution drop bottle
Plug, remaining silver nitrate solution volume reading in drop bottle, is denoted as V after record titration2, you can calculate the nitre with halogen acid gas reaction
The volumetric usage of sour silver：V=V2-V1.Therefore 1g is electric（Line）The amount n of the halogen acid gas of cable burning releaseHXFor（Unit：mol/g）：
nHX = (V·10-3·MAg+)（VAlways/ VSample)/m=0.001V
In formula：
M：Electricity（Line）The quality of cable sample, 1g；
VSample：For the liquor capacity of drop reaction, 100ml；
VAlways：Overall solution volume in measuring bottle, 1000ml；
MAg+：Silver nitrate solution molar concentration, 0.1mol/L；
V：Unit：ml.
Claims (7)
1. a kind of method for measuring cable fire release total amount of halogen acid gas, its determination step are as follows：
Step 1：Various experimental apparatus are cleaned up with distilled water；
Step 2：Surveyed sample of cable is precisely weighed, is subsequently placed in the combustion tube of tubular heating furnace and heats, then sample is burnt
The halogen acid gas of release are imported in the wash bottle equipped with sodium hydroxide solution and fully absorbed, and are measured with PH test paper；
Step 3：Solution in wash bottle is all moved into a certain amount of measuring bottles by connecting tube, and with distilled water flushing wash bottle,
The terminal of connecting tube and combustion tube, while flushing liquor is also poured into measuring bottle, then solution is appended in measuring bottle to one with distilled water
It is quantitative；
Step 4：Poured into a certain amount of solution in measuring cup taken amount bottle in beaker, then clean measuring cup 2-3 times with distilled water, will cleaned
The filtrate remained in measuring cup is poured into beaker, is fully shaken up；
Step 5：Into beaker plus 3~5 drip potassium chromates, make the solution in beaker in light yellow；
Step 6：Beaker is placed in the dropper of rack for test tube in the following, preparing titration；
Before titration, the silver nitrate solution drop bottle initial volume reading on rack for test tube is first recorded, is denoted as V1, open magnetic stirrer pair
Solution in beaker is stirred, appropriate to decontrol rack for test tube silver nitrate solution drop bottle cock, makes silver ion fully anti-with halogen ion
Should, form yellow-white precipitation；It is terminal that pink, which has just occurred, in the solution being persistently titrated in beaker, tightens silver nitrate solution drop bottle
Cock, records remaining silver nitrate solution volume reading in drop bottle at this time, is denoted as V2, you can calculate the nitric acid with halogen ion reaction
The volumetric usage V of silver：V=V2-V1, wherein V, V2、V1Unit：ml；The halogen acid gas amount of cable burning release is counted as follows
Calculate：
nHX = (V·10-3·MAg+)（VAlways/ VSample)/m
In formula：nHX：The halogen acid gas amount of cable burning release, unit：mol；
VSample：For the liquor capacity of drop reaction, unit：ml；
VAlways：Overall solution volume in measuring bottle, unit：ml；
MAg+：Silver nitrate solution molar concentration, unit：mol/L；
V：With the volume of the silver nitrate solution of halogen acid gas reaction, unit：ml；
m:The quality of cable, unit：g.
A kind of 2. method for measuring cable fire release total amount of halogen acid gas according to claim 1, it is characterised in that
In step 2,1g ± 0.1mg cable samples will be precisely weighed and be placed in the combustion tube of tubular heating furnace, then release sample burning
The halogen acid gas put are imported in the wash bottle equipped with 200mL sodium hydroxide solutions and fully absorbed, then are measured with PH test paper, it is desirable to this
When solution pH value be 7-8.
A kind of 3. method for measuring cable fire release total amount of halogen acid gas according to claim 2, it is characterised in that hydrogen
The molar concentration of sodium hydroxide solution is 0.1 mol/L.
A kind of 4. method for measuring cable fire release total amount of halogen acid gas according to claim 3, it is characterised in that
In step 3, then by the sodium hydroxide solution in wash bottle by connecting tube all move into it is a certain amount of be 1000mL measuring bottles in, and with steaming
Distilled water rinses the terminal of wash bottle, connecting tube and combustion tube, while flushing liquor is also poured into measuring bottle, is then appended to distilled water
It is 1000mL that solution is a certain amount of in measuring bottle.
A kind of 5. method for measuring cable fire release total amount of halogen acid gas according to claim 1, it is characterised in that
It is 100ml with a certain amount of solution in measuring cup taken amount bottle in step 4.
A kind of 6. method for measuring cable fire release total amount of halogen acid gas according to claim 1, it is characterised in that
In step 5, the concentration of potassium chromate is 5%, i.e. 5g potassium chromates are dissolved in 95mL distilled water.
A kind of 7. method for measuring cable fire release total amount of halogen acid gas according to claim 1, it is characterised in that
In step 6, silver nitrate solution molar concentration is 0.1 mol/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711115387.5A CN107907626A (en) | 2017-11-13 | 2017-11-13 | A kind of method for measuring cable fire release total amount of halogen acid gas |
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| CN201711115387.5A CN107907626A (en) | 2017-11-13 | 2017-11-13 | A kind of method for measuring cable fire release total amount of halogen acid gas |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09264861A (en) * | 1996-03-29 | 1997-10-07 | Ngk Insulators Ltd | Method and device for measuring gas concentration |
| CN1731168A (en) * | 2005-08-10 | 2006-02-08 | 福建南平太阳电缆股份有限公司 | Method for measuring general quantity of released gas during cable material combustion |
| CN102914537A (en) * | 2012-10-19 | 2013-02-06 | 河北省首钢迁安钢铁有限责任公司 | Method for determining chlorine ion content in coal gas |
| CN105842387A (en) * | 2015-01-12 | 2016-08-10 | 内蒙古包钢钢联股份有限公司 | Method for measuring chloride ions in iron oxide powder through precipitation titration |
-
2017
- 2017-11-13 CN CN201711115387.5A patent/CN107907626A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09264861A (en) * | 1996-03-29 | 1997-10-07 | Ngk Insulators Ltd | Method and device for measuring gas concentration |
| CN1731168A (en) * | 2005-08-10 | 2006-02-08 | 福建南平太阳电缆股份有限公司 | Method for measuring general quantity of released gas during cable material combustion |
| CN102914537A (en) * | 2012-10-19 | 2013-02-06 | 河北省首钢迁安钢铁有限责任公司 | Method for determining chlorine ion content in coal gas |
| CN105842387A (en) * | 2015-01-12 | 2016-08-10 | 内蒙古包钢钢联股份有限公司 | Method for measuring chloride ions in iron oxide powder through precipitation titration |
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Application publication date: 20180413 |