CN110208456A - The detection method of sodium thiosulfate content in two hydration hexa-methylene -1,6- bisthiosulfate disodium salts - Google Patents
The detection method of sodium thiosulfate content in two hydration hexa-methylene -1,6- bisthiosulfate disodium salts Download PDFInfo
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Abstract
The present invention provides the detection methods of sodium thiosulfate content in two hydration hexa-methylene -1,6- bisthiosulfate disodium salts, are first measured to chloride ion content in HTS sample to be checked, avoid influence of the chloride ion to testing result.When being pre-processed to measuring samples, silver nitrate solution, dust technology additional amount be excess, dust technology decomposes the sodium thiosulfate in sample, it is ensured that silver nitrate only reacted with the chloride ion in HTS.After removing interference component, using easy argentometry can accurate detection go out the content of sodium thiosulfate in sample.Detection method is easy to operate without cumbersome preprocessing process, at low cost, sufficiently eliminates the interference component in iodimetric titration detection process, and testing result is accurate, is suitble to large-scale promotion application.
Description
Technical field
The invention belongs to defects inspecting technical fields, particularly belong to two hydration hexa-methylene -1,6- bisthiosulfate disodiums
The detection method of sodium thiosulfate content in salt (HTS) product.
Background technique
Anti-recovery agent two is hydrated hexa-methylene -1,6- bisthiosulfate disodium salt, hereinafter referred to as HTS, its change
Formula is C6H12Na2O6S4·2H2O, molal weight 390.43.Its structural formula is as follows, containing there are two sub- in self structure
Sulfate radical:
HTS is widely used in rubber materials as rubber chemicals, the thermal stability of rubber is significantly improved, in day
HTS is added in right rubber sulfenamide vulcanizing system, heat-staple C-C cross-bond can be generated in sulfidation, C-C is handed over
Connection key can compensate for the polysulfide bond lost by recovery, chain rupture, form not only sulfur-bearing but also carbon containing compound cross-bond, be product
Superior flexibility, heat-resistant aging, dynamic fatigue durability are provided, and effectively inhibits the precipitation of compounding agent, improve stress at definite elongation.
In addition, being alternatively arranged as a kind of promotor to enhance rubber and cross the bonding retentivity between brass all-steel cord.
In the prior art, sodium thiosulfate and 1 are industrially used, the synthetic method that 6- dichloro hexane reacts produces HTS,
Reaction equation is as follows:
2Na2S2O3+Cl-(CH2)6-CL→NaO3SS-(CH2)6-SSO3Na+2NaCl
As can be seen from the above formula that there are unreacted sodium thiosulfate and sodium chloride byproduct, HTS in reaction product
The maximum difficult point of Indexs measure is the detection of sodium thiosulfate in product, this is also the product slowly without putting into effect national standard
Main cause.The presence of sodium thiosulfate seriously affects the performance of sizing material, therefore in production by the content of sodium thiosulfate
Control 1.0% hereinafter, and accurately measure the content of sodium thiosulfate in HTS, to judging properties of rubber important in inhibiting.
In some company standards, iodimetric titration is used to the measuring method of sodium thiosulfate.Iodimetric titration although have it is easy to operate,
Advantage at low cost, but can be seen that HTS from HTS structural formula and itself have inferior sulfate radical structure, it can send out with iodine
Raw reaction, therefore if directlying adopt iodometric determination, the accuracy of testing result must be will affect.Therefore, thiosulfuric acid in HTS
The precise measurement of sodium is a problem to be solved always.
Summary of the invention
The inspection of sodium thiosulfate content in two hydrations hexa-methylene -1,6- bisthiosulfate disodium salt provided by the present invention
Survey method can effectively avoid influence of the HTS to testing result itself, and easy to operate, and testing result is more accurate.
The detection method of sodium thiosulfate content, feature in two hydration hexa-methylene -1,6- bisthiosulfate disodium salts
It is, includes the following steps:
Step 1: blank titration
10ml water is taken, the silver nitrate solution containing 0.0845g silver nitrate is added, 2ml glycerine is added and is aggressively shaken, is added
Dilute nitric acid solution, the amount of addition and the volume ratio of water are 1-1.5, and indicator is added, with ammonium thiocyanate solution titration end-point, record
The volume V of ammonium thiocyanate consumption2, as blank control；
Step 2: sample pretreatment:
It takes 0.2-1.0g HTS measuring samples to be dissolved in water and forms aqueous solution, the mass ratio of HTS measuring samples and water is 1:50-
1:150；Later by HTS measuring samples solution, 10-30ml dilute nitric acid solution (concentration 10%) and silver nitrate solution, wherein nitre
The weight of the silver nitrate contained in sour silver solution and the weight ratio of HTS measuring samples are as follows: 1:1-1:10；In slow heating, stirring
Lower mixing 10-15min；Obtain reserve liquid 1；
Step 3: chloride ion content (in terms of sodium chloride) in measurement HTS measuring samples:
Reserve liquid 1 is taken, glycerine is added, is aggressively shaken, indicator is added, to terminal with ammonium thiocyanate titration, records sulphur
The volume V of ammonium cyanate consumption3, the mass fraction of sodium chloride in sample are as follows:
In formula (2)
CNH4SCN- ammonium thiocyanate concentration, mol/l
mSample- sample quality, g
MNaclThe molal weight of-sodium chloride, 58.44
CNH4SCN- ammonium thiocyanate standard solution molar concentration, mol/l
V2The volume of the ammonium thiocyanate solution consumed in-blank assay
V3The volume of the ammonium thiocyanate solution consumed in-sample continuous mode
Step 4: argentometry measures sodium thiosulfate content in HTS measuring samples:
Separately 0.2-1.0g HTS measuring samples is taken to be dissolved in 10-30ml water, add indicator, dripped with silver nitrate titer (C)
Determine to terminal；After reaching titration end-point, sodium thiosulfate content ω % is calculated according to the following formula；
In formula: ω %-sodium thiosulfate content, %
ωNaClThe content of sodium chloride, % in-sample
C-silver nitrate titer concentration, mol/L
V-silver nitrate titer volume, L
The grams of the alleged material of m-, g
The relative molecular mass of 58.44-sodium chloride
248.17-sodium thiosulfate (Na2S2O3·5H2O relative molecular mass).
Preferably, indicator used is ammonium ferric sulfate in the step 1 and step 3, dosage 1ml, and titration end-point is
There is stable pale red；Indicator used is saturation potassium chromate solution in the step 4, and titration end-point is brick red occur
Color.
Preferably, the step 1 and step 2 silver nitrate solution concentration are 0.1mol/L.
Reaction mechanism of the invention are as follows:
In measuring HTS measuring samples when sodium chloride content:
Firstly, the sodium thiosulfate in sample is decomposed；It dissolves a sample in suitable quantity of water, excess nitric acid, excess is added
Silver nitrate, is heating slowly facilitated dust technology to decompose the sodium thiosulfate in sample, because sodium thiosulfate and sodium chloride all can be with
Nitric acid silver reaction, so sodium thiosulfate to be decomposed to the measurement for interfering sodium chloride content to avoid it；
Secondly, solution clarification, it is silver nitride precipitation that a small amount of white precipitate, which is arranged, at bottom after sodium thiosulfate decomposes；
Glycerine is added to coat silver chlorate, prevents precipitating dissolution equilibrium mobile to the direction of dissolution；
Finally, ammonium ferric sulfate indicator is added, titrated with ammonium thiocyanate solution, at this point, in ammonium thiocyanate and solution
Remaining silver nitrate is reacted.
When measuring sodium thiosulfate content in HTS measuring samples:
It takes sample to be dissolved in suitable quantity of water, potassium chromate solution indicator is added, is titrated to appearance with silver nitrate titer (C)
Brick-red is terminal；In titration process, silver nitrate is not only reacted with the sodium chloride in sample but also is reacted with sodium thiosulfate, and 1mol
Sodium thiosulfate and 2mol nitric acid silver reaction.Therefore the mole for consuming silver nitrate is the thio of+2 times of mole of sodium chloride
The mole of sodium sulphate.(2) " 2 " in formula on denominator are from 1mol sodium thiosulfate and 2mol nitric acid silver reaction；What is expressed is the mole that silver nitrate mole deducts sodium chloride.
Beneficial effects of the present invention:
The new method that sodium thiosulfate content detects in the present invention, new thinking is provided for HTS product testing, is solved
It is difficult to the problem overcome always in sodium thiosulfate detection in HTS.The principle of the invention is: first to chloride ion in HTS sample to be checked
Content is measured, and avoids influence of the chloride ion to testing result.It is silver nitrate solution, dilute when being pre-processed to measuring samples
The additional amount of nitric acid is excess, and dust technology decomposes the sodium thiosulfate in sample, it is ensured that silver nitrate only with the chlorine in HTS from
Son is reacted.After removing interference component, using easy argentometry can accurate detection go out sodium thiosulfate in sample
Content.
Detection method is easy to operate without cumbersome preprocessing process, at low cost, sufficiently eliminates iodimetric titration detection
Interference component in the process, testing result is accurate, is suitble to large-scale promotion application.
Specific embodiment
Embodiment 1
By sodium thiosulfate content in two hydrations hexa-methylene -1,6- bisthiosulfate disodium salt provided by the present invention
(the sodium chloride standard of certain mass is added in detection method, the hypo solution for measuring known concentration in the solution
Product), to verify to detection method, steps are as follows:
Step 1: the configuration and calibration of solution:
Ammonium ferric sulfate indicator: about 5g Ammonium ferric sulfate dodecahyrate is taken to be dissolved in the distilled water that a little nitric acid is added dropwise in 50ml
In.
Dilute nitric acid solution: with concentrated nitric acid and distilled water with volume ratio 1:3 mixing.
The preparation and calibration of silver nitrate solution:
Prepare: precise 8.50g silver nitrate is dissolved in distilled water, carries out constant volume using 500ml brown volumetric flask,
Obtain the silver nitrate solution that concentration is about 0.1mol/L；
Calibration: precise m is the NaCl after 0.115g roasting in 50ml conical flask, deionized water is added its is molten
Solution.Two drop potassium chromate solutions are added into conical flask as indicator, it is titrated with configured silver nitrate solution, when
Occurs brick-red precipitating in conical flask, i.e., explanation reaches titration end-point, parallel titration 3 times, at this point, the average body of consumption silver nitrate
V is accumulated as 18.7ml, if the concentration of silver nitrate is C mol/L, the actual concentration of silver nitrate is calculated according to following equation.According to this
Method, the concentration for acquiring silver nitrate is 0.105mol/L.
V-silver nitrate consumption (ml)；
C-silver nitrate concentration (mol/L)；
M-sodium chloride quality (g).
The preparation and calibration of ammonium thiocyanate solution:
Configuration: it takes 2g ammonium thiocyanate to be dissolved in distilled water, 1L is settled in volumetric flask, obtain about 0.026mol/L's
Ammonium thiocyanate solution.
Calibration: ammonium thiocyanate solution calibration: the sodium chloride standard that 5ml 0.05mol/L is added in 100ml conical flask is molten
Then the silver nitrate solution of 5ml 0.105mol/L is added in liquid, 2ml glycerine is added and is aggressively shaken, 10ml nitric acid solution is added,
1ml ammonium ferric sulfate indicator is added, is titrated to ammonium thiocyanate solution and stable pale red occurs, record ammonium thiocyanate consumption
Volume V1.Same method does not take chlorination sodium standard solution, and the silver nitrate with ammonium thiocyanate titration 5ml 0.105mol/L is molten
Liquid records the volume V of ammonium thiocyanate consumption as blank control2.In this way, parallel titration 3 times, average external volume V1For
19.1ml, average external volume V2For 29.1ml.If the concentration of ammonium thiocyanate is CNH4SCNMol/L calculates sulphur according to following equation
The actual concentration of ammonium cyanate.The concentration for acquiring ammonium thiocyanate is 0.025mol/L.
In formula
CNaClThe concentration of-chlorination sodium standard solution, mol/l
CNH4SCNThe concentration of-ammonium thiocyanate solution, mol/l
V1The volume of the ammonium thiocyanate solution of-sodium chloride-containing reference solution consumption, ml
V2The volume of-the ammonium thiocyanate solution that sodium chloride-containing reference solution does not consume, ml
5-silver nitrate volumes, ml
Step 2: chloride content measurement (in terms of sodium chloride): weighing the sodium chloride standard items of 0.002g and contain 0.004g
The standard solution of sodium thiosulfate mixes, and is dissolved in 30ml water.10ml dilute nitric acid solution (10%) first is added, 5ml is added
The silver nitrate solution of 0.105mol/L is slowly heated solution to be measured, and until solution becomes clear, colorless by muddiness, bottom has
A small amount of white precipitate.2ml glycerine is added after solution is cooling, is aggressively shaken, 1ml ammonium ferric sulfate indicator is added, uses thiocyanic acid
Ammonium, which is titrated to, there is stable pale red, the volume V of record ammonium thiocyanate consumption3, the mass fraction of sodium chloride is in sample
ωNacl, m takes 0.006g herein, is 33.3% according to the real quality score that following equation calculates sodium chloride, with true value one
It causes.
In formula:
CNH4SCN- ammonium thiocyanate concentration, mol/l
mSample- sample quality, g
MNaclThe molal weight of-sodium chloride, 58.44
CNH4SCN- ammonium thiocyanate standard solution molar concentration, mol/l
Step 3: the measurement of sodium thiosulfate content: weighing the sodium chloride standard items of 0.002g and contains the thio sulphur of 0.004g
The standard solution of sour sodium mixes, and is dissolved in 30ml water.2 drop saturation potassium chromate solutions are added dropwise, are titrated with silver nitrate titer (C)
Brick-red to appearance is terminal, records consumed titer volume V, parallel to titrate 3 times, the average external volume of silver nitrate used is
0.63ml.Substitute into formula calculate sodium thiosulfate content be 66.6%.
In formula: ω %-sodium thiosulfate content, %
ωNaCThe content of sodium chloride, % in-sample
C-silver nitrate titer concentration, mol/L
V-silver nitrate titer volume, L
The grams of the alleged material of m-, g
By calculating, the mass fraction of the sodium chloride detected and the content of sodium thiosulfate are consistent with true value.It says
The measuring method of bright sodium thiosulfate provided by the present invention be it is feasible, the addition of the reagents such as silver nitrate and ammonium thiocyanate will not
Influence the accuracy of detection sodium thiosulfate.
Embodiment 2
The content of sodium thiosulfate in unknown HTS product is measured, steps are as follows:
Step 1 is identical as the step in embodiment 1；Prepare ammonium ferric sulfate indicator, concentrated nitric acid and distilled water with volume ratio
Dilute nitric acid solution that 1:3 is obtained, 0.1mol/L silver nitrate solution, 0.025mol/L ammonium thiocyanate solution；
Step 2: chloride content measure (in terms of sodium chloride): in 100ml conical flask be added 0.2010g HTS sample and
First 10ml dilute nitric acid solution (10%) is added in 30ml ultra-pure water solution, and the silver nitrate solution of 5ml 0.1mol/L is added (if sample
There is a small amount of sodium thiosulfate to remain in product, solution will become orange red or black precipitate occurs).It is slowly heated solution to be measured, directly
Until solution becomes clear, colorless by muddiness, a small amount of white precipitate is arranged at bottom.2ml glycerine is added after solution is cooling, acutely
It shakes, 1ml ammonium ferric sulfate indicator is added, be titrated to ammonium thiocyanate and stable pale red occur, record ammonium thiocyanate consumption
Volume V3, the mass fraction of sodium chloride is ω in sampleNacl, the real quality score of sodium chloride is calculated according to following equation
It is 0.9%.
In formula
CNH4SCN- ammonium thiocyanate concentration, mol/l
mSample- sample quality, g
MNaclThe molal weight of-sodium chloride, 58.44
CNH4SCN- ammonium thiocyanate standard solution molar concentration, mol/l
Step 3: the measurement of sodium thiosulfate content: accurately weighing 0.2010g product, and 10ml water is added to dissolve, then plus 2 drops it is full
And potassium chromate solution, it is titrated to silver nitrate titer (C) and occurs brick-red being terminal, record consumed titer volume V,
Parallel titration 3 times, the average external volume V of silver nitrate used are 0.60ml.
In formula: ω %-sodium thiosulfate content, %
ωNaClThe content of sodium chloride, % in-sample
C-silver nitrate titer concentration, mol/L
V-silver nitrate titer volume, L
The grams of the alleged material of m-, g
It substitutes into formula to calculate, the content ω % of the sodium thiosulfate in sample is 2%.
Embodiment 3
HTS sample in 0.2217g embodiment 2 is weighed, the hypo solution that known content is 0.004g is mixed into, as
Sample to be tested.The relationship of comparative measurements value and theoretical value, so that the accuracy to the method for inspection of the present invention is further verified.
Step 1 is identical as the step in embodiment 1；Prepare ammonium ferric sulfate indicator, concentrated nitric acid and distilled water with volume ratio
Dilute nitric acid solution that 1:3 is obtained, 0.1mol/L silver nitrate solution, 0.025mol/L ammonium thiocyanate solution；
Step 2: chloride content measurement (in terms of sodium chloride): adding 10ml water to dissolve sample to be tested 0.2257g, be first added
The silver nitrate solution of 5ml 0.1mol/L is added (if there is a small amount of sodium thiosulfate residual in sample in 10ml nitric acid solution (10%)
It stays, solution will become orange red or black precipitate occurs).It is slowly heated solution to be measured, until solution becomes transparent nothing by muddiness
Until color, a small amount of white precipitate is arranged at bottom.2ml glycerine is added after solution is cooling, is aggressively shaken, 1ml ammonium ferric sulfate is added and refers to
Show agent, is titrated to ammonium thiocyanate and stable pale red occur, parallel titration 3 times, the average external volume of record ammonium thiocyanate consumption
V3, the mass fraction of sodium chloride is ω in sampleNacl, it is 0.9% according to the mass fraction that following equation calculates sodium chloride.
In formula
CNH4SCN- ammonium thiocyanate concentration, mol/l
mSample- sample quality, g
MNaclThe molal weight of-sodium chloride, 58.44
CNH4SCN- ammonium thiocyanate standard solution molar concentration, mol/l
Step 3: the measurement of sodium thiosulfate content: adding 10ml to dissolve sample to be tested 0.2257g, then plus 2 drop saturation chromium
Sour potassium solution is titrated to silver nitrate titer (C) and occurs brick-red being terminal, records consumed titer volume V, in parallel
Titration 3 times, the average external volume of silver nitrate used are 0.97ml.
In formula: ω %-sodium thiosulfate content, %
ωNaClThe content of sodium chloride, % in %-sample
C-silver nitrate titer concentration, mol/L
V-silver nitrate titer volume, L
The grams of the alleged material of m-, g
By calculating, the content of sodium thiosulfate is 3.7% in sample.The theoretical content of sodium thiosulfate in measuring samples
For (2%*0.2217+0.004)/0.2257 × 100%=3.7%.It can thus be seen that the sodium thiosulfate that detection obtains
Content and the theoretical content difference of sodium thiosulfate in measuring samples are little, illustrate test method of the present invention to sodium thiosulfate
Measurement is feasible.
Further, the HTS sample that the sodium thiosulfate content of above-mentioned different quality is 2% is taken respectively, respectively thereto
The sodium thiosulfate for mixing different quality, as measuring samples.Repeat above-mentioned detecting step, comparative measurements value and theoretical value, knot
Fruit see the table below 1:
Table 1
From the data of table 1 it can be seen that the relative deviation of the test result of multiple groups test is respectively less than 2.0%, measurement result
Favorable reproducibility, and after the different sodium thiosulfate contents of incorporation, measurement result is close with theoretical value, illustrates test method pair of the present invention
The measurement of sodium thiosulfate is feasible.
Comparative example 1
With the sodium thiosulfate in iodometric determination HTS.
The HTS sterling (without containing sodium chloride, thiosulfuric acid sodium impurity) for taking different quality respectively, mixes not thereto respectively
The sodium thiosulfate of homogenous quantities, as measuring samples.Each measuring samples are detected by the following method, the results are shown in Table lattice 2,
Specific step is as follows:
Step 1:0.01mol/L hypo solution is prepared and calibration
It prepares
Weigh 2.6g sodium thiosulfate (Na2S2O3·5H2O), 0.02g natrium carbonicum calcinatum is added, is dissolved in 1000mL pure water
In, 10min is slowly boiled, it is cooling, it is stored in brown reagent bottle.
Calibration
0.18g is weighed in 120 DEG C of ± 2 DEG C of dryings to the working standard reagent potassium bichromate of constant weight, is placed in iodine flask, it is molten
In 25mL water, 2g potassium iodide and 20mL sulfuric acid solution (20%) is added to shake up, places 10min in dark place.Add (15 DEG C -20 of 15mL water
DEG C), titrated with prepared hypo solution, when nearly terminal (when the color of solution is changed into light yellow by brownish red) plus
1mL starch indicator liquid (10g/L), continuing to be titrated to solution becomes bright green, as titration end-point from blue, titrates 3 in parallel
Secondary, the average external volume for consuming hypo solution is V1.Blank assay is done simultaneously, the volume for consuming hypo solution is
V2。
It calculates
The concentration values of sodium thiosulfate standard titration solution are indicated with mol/L, are calculated as follows:
In formula:
M-potassium bichromate quality, g
V1The volume of-hypo solution, mL
V2The volume of-blank assay hypo solution, mL
M-potassium bichromate molal weight, g/moL [M (1/6K2Cr2O7)=49.031
Step 2:c (1/2I2)=0.01mol/L iodine standard titration solution is prepared and calibration
It prepares
1.3g iodine and 3.5g potassium iodide are weighed, is dissolved in 100mL water, is diluted to 1000mL, shake up, be stored in brown bottle
In.
Calibration
The prepared iodine solution of 35mL-40mL is measured, volume is denoted as V3, be placed in iodine flask, add 150mL water (15 DEG C-
20 DEG C), with sodium thiosulfate standard titration solution [c (Na2S2O3)=0.01mol/L] titration, when nearly terminal adds 2mL starch to refer to
Show liquid (10g/L), continues to be titrated to the disappearance of solution blue, parallel titration 3 times, the average external volume for consuming hypo solution is
V1.The blank test of the consumed iodine of water is done simultaneously: being taken 250mL water (15 DEG C -20 DEG C), is added the prepared iodine of 0.05mL-0.20mL
Solution and 2mL starch indicator solution (10g/L), the volume of iodine solution are denoted as V4, with sodium thiosulfate standard titration solution [c
(Na2S2O3)=0.01mol/L] it is titrated to the disappearance of solution blue, the volume for consuming hypo solution is V2。
It calculates
Concentration [c (the 1/2I of iodine standard titration solution2)], numerical value is indicated with mol/L, it is calculated as follows:
In formula:
V1The volume of-sodium thiosulfate standard titration solution, mL
V2The volume of-blank assay sodium thiosulfate standard solution, mL
C1The concentration of-sodium thiosulfate standard solution, mol/L
V3The volume of-iodine solution, mL
V4The volume of iodine solution, mL in-blank assay
Step 3: the measurement of sodium thiosulfate content
Measurement
It weighs 3.0g HTS measuring samples, claims quasi- to 0.0001g, be dissolved in 70mL without in the water of carbon dioxide, with iodine standard
Solution [c (1/2I2)]=0.01mol/L titration to terminal when, add 3mL starch indicator solution (10g/L), continue to be titrated to solution at
Blue (1min is non-discolouring), parallel titration 3 times, the average external volume of consumption iodine standard titration solution volume are V.
It calculates
The mass fraction ω of sodium thiosulfate, numerical value is indicated with %, is calculated as follows:
In formula:
V-iodine standard titration solution volume, mL
C-iodine standard titration solution concentration, mol/L
M-sample mass, g
M-sodium thiosulfate molal weight
The measured value that will test is compared with theoretical value, as a result see the table below 2:
2 experimental data of table
In the measuring samples that traditional iodimetric titration measures it can be seen from comparative example 1, the sodium thiosulfate content that measures with
The theoretical value difference of the sodium thiosulfate contained is larger, and iodimetric titration is not suitable for measuring the content of sodium thiosulfate in HTS.Cause
For in HTS sample, not only sodium thiosulfate is reacted in elemental iodine, and the effective component two in HTS is hydrated hexa-methylene -1,6-
Similar reaction can equally occur with elemental iodine for bisthiosulfate disodium salt, influence measurement result.
Claims (3)
1. the detection method of sodium thiosulfate content, feature exist in two hydration hexa-methylene -1,6- bisthiosulfate disodium salts
In including the following steps:
Step 1: blank titration
10ml water is taken, the silver nitrate solution containing 0.0845g silver nitrate is added, 2ml glycerine is added and is aggressively shaken, dilute nitre is added
Acid solution, the amount of addition and the volume ratio of water are 1-1.5, and indicator is added, and with ammonium thiocyanate solution titration end-point, record sulphur cyanogen
The volume V of sour ammonium consumption2, as blank control；
Step 2: sample pretreatment:
It takes 0.2-1.0g HTS measuring samples to be dissolved in water and forms aqueous solution, the mass ratio of HTS measuring samples and water is 1:50-1:
150；Later by HTS measuring samples solution, 10-30ml dilute nitric acid solution (concentration 10%) and silver nitrate solution, wherein nitric acid
The weight of the silver nitrate contained in silver-colored solution and the weight ratio of HTS measuring samples are as follows: 1:1-1:10；Under slow heating, stirring
Mix 10-15min；Obtain reserve liquid 1；
Step 3: chloride ion content (in terms of sodium chloride) in measurement HTS measuring samples:
Reserve liquid 1 is taken, glycerine is added, is aggressively shaken, indicator is added, to terminal with ammonium thiocyanate titration, records thiocyanic acid
The volume V of ammonium consumption3, the mass fraction of sodium chloride in sample are as follows:
In formula (2)
CNH4SCN- ammonium thiocyanate concentration, mol/l
mSample- sample quality, g
MNaclThe molal weight of-sodium chloride, 58.44
CNH4SCN- ammonium thiocyanate standard solution molar concentration, mol/l
V2The volume of the ammonium thiocyanate solution consumed in-blank assay
V3The volume of the ammonium thiocyanate solution consumed in-sample continuous mode
Step 4: argentometry measures sodium thiosulfate content in HTS measuring samples:
Separately 0.2-1.0g HTS measuring samples is taken to be dissolved in 10-30ml water, adds indicator, be titrated to silver nitrate titer (C)
Terminal；After reaching titration end-point, sodium thiosulfate content ω % is calculated according to the following formula；
In formula: ω %-sodium thiosulfate content, %
ωNaClThe content of sodium chloride, % in-sample
C-silver nitrate titer concentration, mol/L
V-silver nitrate titer volume, L
The grams of the alleged material of m-, g
The relative molecular mass of 58.44-sodium chloride
248.17-sodium thiosulfate (Na2S2O3·5H2O relative molecular mass).
2. sodium thiosulfate content in two hydrations hexa-methylene -1,6- bisthiosulfate disodium salt according to claim 1
Detection method, which is characterized in that indicator used is ammonium ferric sulfate, dosage 1ml, titration in the step 1 and step 3
Terminal is stable pale red occur；Indicator used is saturation potassium chromate solution in the step 4, and titration end-point is to occur
It is brick-red.
3. sodium thiosulfate content in two hydrations hexa-methylene -1,6- bisthiosulfate disodium salt according to claim 1
Detection method, which is characterized in that silver nitrate solution concentration used is 0.1mol/L in the step 1 and step 2.
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