GOST 6689.10-92
GOST 6689.10−92 Nickel, alloys Nickel and copper-Nickel. Methods for determination of carbon
GOST 6689.10−92
Group B59
STATE STANDARD OF THE USSR
NICKEL, ALLOYS NICKEL AND COPPER-NICKEL
Methods for determination of carbon
Nickel, nickel and copper-nickel alloys. Methods for the determination of carbon
AXTU 1709
Date of introduction 1993−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of metallurgy of the USSR
DEVELOPERS
V. N. Fedorov, Y. M. Leybov, Boris Krasnov, A. N. Bulanova, I. A. Vorobyev
2. APPROVED AND promulgated by the Decree of Committee of standardization and Metrology of the USSR from
3. REPLACE GOST 6689.10−80
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
The number of the paragraph, subparagraph, section |
| GOST 8.315−91 |
2.5.3; 3.5.3; 4.4.3 |
| GOST 435−77 |
2.2 |
| GOST 492−73 |
Chapeau |
| GOST 859−78 |
2.2; 3.2 |
| GOST 4107−78 |
2.2 |
| GOST 4108−72 |
2.2 |
| GOST 4204−77 |
2.2 |
| GOST 4328−77 |
2.2 |
| GOST 5583−78 |
2.2; 4.2 |
| GOST 6689.1−92 |
Sec. 1 |
| GOST 10929−76 |
2.2 |
| GOST 18300−87 |
2.2; 4.2 |
| GOST 19241−80 |
Chapeau |
| GOST 20490−75 |
2.2; 3.2 |
| GOST 22300−76 |
4.2 |
| GOST 25086−87 |
Sec. 1; 2.5.3; 3.5.3; 4.4.3 |
| THAT 6−09−3523−74 |
4.2 |
| THAT 6−09−2705−78 |
4.2 |
| THAT 6−09−3000−78 |
4.2 |
| THAT 48−19−57−78 |
4−2 |
This standard specifies potentiometric (when the mass fraction of carbon from 0.002 to 0.3%), volumetric (when the mass fraction of the carbon from 0.01 to 0.3%) methods and the method using automatic and semiautomatic analyzers (when the mass fraction of carbon from 0.002 to 0.3%) for the determination of carbon in Nickel and copper-Nickel alloys according to GOST 492* and GOST 19241.
______________
* On the territory of the Russian Federation GOST 492−2006. — Note the manufacturer’s database.
1. GENERAL REQUIREMENTS
General requirements for methods of analysis GOST 25086 with the addition of sec. 1 GOST 6689.1.
2. POTENTIOMETRIC METHOD FOR DETERMINATION OF CARBON
2.1. The essence of the method
The method is based on burning a sample of the alloy in a current of oxygen at 1350−1400 °C, the absorption of generated carbon dioxide with a solution of barium chloride and hydroxide and barium titration of this solution with a hydroxide of barium to its original pH value.
2.2. Apparatus, reagents and solutions
Installation for the determination of carbon (Fig.1) consists of the oxygen cylinder 1 or coloradobased; U-shaped tube with soda lime 2; vessel with 1 mol/DM3 sulfuric acid, the vessel with a solution (40 g/DM
) sodium hydroxide 4; apparatus for the combustion of carbon monoxide 5; vessel with a solution (50 g/DM
) hydroxide barium 6; vessel with 2 mol/DM
sulfuric acid solution 7; constipation (tube) tube for burning 8; refrigerators, 9, 12; porcelain tube for burning 10 with a diameter of 18−22 mm (handset before use should be calcined at 1200 °C); horizontal electric tubular furnace 11 with automatic temperature control up to 1400 °C; the absorption vessel with manganese dioxide 13; of the vessel for pressure equalization 14; three-way valve 15; a tube with electrodes 16 (Fig.2); microburette with a solution of barium hydroxide 17; galvanometer 18; compensation schemes 19 (Fig.3).
Damn.1
Damn.2
Damn.3
Tube with electrodes (Fig.2) consists of a glass tube 1; silver chloride electrode 2; the tubes 3; sealed platinum electrode 4; rubber o ring 5; a glass filter 6; plug covering glass filter 7; gazoprovoda tube 8.
Compensation scheme (Fig.3) consists of a tube 1 of solid glass with a diameter of 6−8 mm; helix 2 from platinum wire with a diameter of 1 mm; variable resistance 3 1.5 Ohm and 4; battery 4 to 6 V.
Copper grade MO according to GOST 859* in the form of fine shavings or sawdust.
______________
* On the territory of the Russian Federation GOST 859−2001, here and hereafter. — Note the manufacturer’s database.
Potassium permanganate according to GOST 20490, a solution of 40 g/DM.
Barium chloride according to GOST 4108.
Manganese sulfate according to GOST 435.
Standard sample for setting the operating mode of the installation. Use the national standard samples: 2146−81 GSO, GSO 838−84п of the bonds 1632−83п of the bonds 1377−82п, GEO 716−84п, GSO 1862−85п, 1862−80 GSO, GSO 1498−83п of the bonds 1609−85п.
Barium hydroxide 8-water according to GOST 4107, a solution of 50 g/DMand the solution for titration. Solution for titration of 5 g of barium hydroxide and 1.4 g of sodium hydroxide dissolved in 1 DM
of boiled water. The solution is mixed, filtered and poured into microburette. All holes in microburette must be replaced by tubes filled with soda lime.
Establish a bulk solution concentration of barium hydroxide: 1 g of a standard sample of Nickel or steel in the form of a small chip placed in a porcelain boat, mixing with 1 g of copper.
A boat placed in a tube for flaring and then do as described in claim 2.4.
Manganese dioxide deposited on the asbestos fiber: 13 g of manganese sulfate dissolved in a small amount of water and this solution is saturated with 90 g of asbestos fibers, pre-calcined at 1000 °C. In a vessel with asbestos and manganese sulfate are added 200 cmof solution of potassium permanganate and boil for 5 minutes Asbestos with precipitated manganese dioxide is filtered off, washed with hot water and dried at 105 °C.
The technical rectified ethyl alcohol according to GOST 18300.
Hydrogen peroxide according to GOST 10929, 30% solution.
Phenolphthalein according to NTD, a solution of 10 g/lin ethanol.
The absorption solution 11 g of barium chloride dissolved in 500 cmsvejeprokipachenna of water, add 5 cm
of ethyl alcohol and 0.5 cm
of hydrogen peroxide solution diluted with water to 1 DM
.
Unglazed porcelain boats, pre-calcined at 1200 °C in flowing oxygen. Boats stored in a desiccator with soda lime or calcium chloride.
Oxygen gas according to GOST 5583.
Sulfuric acid according to GOST 4204, 2 mol/DMsolution.
Sodium hydroxide according to GOST 4328 and a solution of 40 g/DM.
The mass concentration of the solution of hydroxide of barium is calculated by the formula
where — mass fraction of carbon in the standard sample, %;
the volume of the solution of barium hydroxide, spent on titration, sm
.
Lime soda with a content of 6−8% moisture.
Calcium chloride for NTD.
2.3. Training equipment
Oven heated to 1350−1400 °C and the tube stoppered. Set the feed rate of the oxygen so that combustion took place with its excess. Vessel to equalize the pressure is lowered, while the absorption tube is filled with a solution. For a cylindrical vessel, make a note of the level of mercury at which the glass Frit begins to flow oxygen. Then the vessel with mercury pick up and set on a tripod.
To the absorption solution was added 3 drops of phenolphthalein solution, 1 cmof a solution of barium hydroxide, mix, and allow oxygen and set the arrow of the galvanometer to zero using the compensation scheme. Turn the three-way tap so that the equipment was connected to the atmosphere, and opens up for burning.
2.4. Analysis
A portion of small chips of alloy weighing 1 g is placed in a porcelain boat and was stirred for 1 g of shavings or sawdust copper. A boat placed in a tube for flaring, the tube closed with a stopper and close the threeway tap.
Vessel to equalize the pressure is lowered. When the mercury in the cylindrical vessel comes to the label (see p.2.3) turn three-way tap connecting pipe for burning the absorption vessel.
As combustion of the sample, the absorption solution is titrated with a solution of barium hydroxide until the return arrow of the galvanometer to its original position. At the end of the burning vessel to align gently raise and stop the titration.
At the same time experiments were conducted with 1 g of copper shavings or sawdust.
2.5. Processing of the results
2.5.1. Mass fraction of carbon in percent is calculated by the formula
where — volume of the solution of barium hydroxide used for the titration of carbon dioxide released during combustion of sample, cm
;
the volume of the solution of barium hydroxide consumed for titration of the solution in the idle experience, cm
;
— mass concentration of a solution of barium hydroxide;
— the weight of the portion of alloy,
2.5.2. Discrepancies in the results of three parallel measurements (rate of convergence) and the results of two tests
(rate of convergence) must not exceed the values of permissible differences given in the table.
| Mass fraction of carbon, % |
The allowable divergence, % | |
| From 0.002 to 0.004 incl. |
0,001 |
0,001 |
| SV. 0,004 «0,006 « |
0,002 |
0,003 |
| «Is 0.006» to 0.012 « |
0,003 |
0,004 |
| «To 0.012» 0,024 « |
0,004 |
0,006 |
| «0,024» 0,05 « |
0,006 |
0,008 |
| «0,05» 0,10 « |
0,008 |
0,01 |
| «To 0.10» to 0.20 « |
0,01 |
0,01 |
| «To 0.20» to 0.30 « |
0,02 |
0,03 |
2.5.3. Control of accuracy of analysis results is guaranteed by the establishing of operating mode according to the State standard samples (p.2.2) approved by GOST 8.315* in accordance with GOST 25086.
______________
* On the territory of the Russian Federation GOST 8.315−97, here and hereafter. — Note the manufacturer’s database.
3. THE VOLUMETRIC METHOD FOR THE DETERMINATION OF CARBON
3.1. The essence of the method
The method is based on burning a sample of the alloy in a current of oxygen at 1350−1400 °C, the absorption of generated carbon dioxide with a solution of potassium hydroxide. The difference between the initial volume of gas and its volume after absorbing the carbon dioxide with a solution of potassium hydroxide find the carbon content.
3.2. Apparatus, reagents and solutions
Setting to define (Fig.4) carbon is composed of 1 oxygen cylinder with reducer or coloradobased; Tishchenko flask with a solution of potassium hydroxide (30%) containing 5% potassium permanganate, 2 and a bottle of 1 mol/DMsulfuric acid solution 3; column of granular potassium hydroxide 4; single-acting crane 5; a porcelain tube 6 an inner diameter of 18−22 mm (handset before use should be calcined at 1300 °C); horizontal electric tube furnace 7 with automatic temperature control up to 1400 °C; the glass ball filter 8 filled with glass wool; glass single tap 9; the detector SEI-1 or SEI-2 10 for NTD.
Damn.4
The detector includes coils of the refrigerator 11; the three-way valve 12; measuring burette (audiometer) 13; equalizing the bottle 14; the absorption vessel with the balloon 15 and the absorption vessel 16.
Copper grade MO according to GOST 859 in the form of fine shavings or sawdust.
Boats unglazed porcelain, preheated at the working temperature in flowing oxygen. Boats are stored in a desiccator with calcium chloride or soda lime.
Standard sample for setting the operating mode of the installation. Use the national standard samples: 2146−81 GSO, GSO 888−84п of the bonds 1774−84п of the bonds 1632−83п, GEO 716 — 84п, GSO 1862−85п of the bonds 1609−85п.
Lime soda with a moisture content of 6−8%.
Potassium chloride for NTD.
Potassium permanganate according to GOST 20490, solution 50 g/lin a solution of 400 g/DM
of potassium hydroxide.
Potassium hydroxide 1 mol/DMsolution.
3.3. Training equipment
When checking for leaks one end of the porcelain tube connecting a rubber hose through cleaning bottles with the balloon, and the second unit go. At the operating temperature of the furnace fill the absorption vessel GOU solution of potassium hydroxide, and the surge flask are placed 400 to 450 cm2% solution of sulfuric acid containing two or three drops of solution of methyl orange.
The color change of methyl orange from red to yellow when working indicates penetration audiometr of the alkali solution from the absorption vessel. In this case, the liquid in eudiometer should be replaced immediately fresh. After each fill surge bottle with fresh liquid it is recommended to make one or two preliminary incineration of batches of Nickel or copper-Nickel alloy to saturate the liquid with carbon dioxide. Otherwise, when the determination of the carbon equalization after filling flasks with fresh liquid first results may be underestimated.
To control the correct operation of the unit before starting work and after every 2−3 hours while you work burn two or three sample standard sample of Nickel or steel with certified carbon content.
3.4. Analysis
A sample of alloy weighing 1 g is placed in a porcelain boat and even layer add 0.5−1 g of copper shavings or sawdust. A boat with suspension and a smoother hook is placed in the most heated portion of the porcelain tube. The end of the tube is closed immediately with a rubber stopper, thus connecting the furnace with an oxygen cylinder and apparatus. 10−20 with electric current of oxygen at a rate of 4−5 bubbles per second.
When burning is completed, the fluid level in audiometry begins to fall and when it reaches almost zero scale divisions stop the flow of oxygen, porcelain disconnect the receiver and remove the boat. The fluid level in audiometry set at the zero scale division, and the liquid level in the surge flask set at the same level with the liquid in eudiometer. The gas mixture is transferred by turning the tap in the sink, making sure that at the top of audiometry was free of gas bubbles.
From the absorption vessel, the remaining gas is again pumped into eudiometer and the operation of absorbing carbon dioxide again.
Turn the tap disconnect audiometer from the sinks. After 1 min of exposure measuring gas volume, which equalizing the bottle is moved vertically along the burette from the bottom up to the position at which the liquid levels in audiometry and surge flask are the same.
By measuring the volume of gas in the burette, record the corresponding scale division. The analysis captures the temperature of the gas in eudiometry and atmospheric pressure on the barometer. Carry out blank with 0.5 or 1 g fine dust as described above.
3.5. Processing of the results
3.5.1. Mass fraction of carbon in percent is calculated by the formula
where the scale parameters of audiometry after absorption of carbon dioxide by combustion of the sample, %;
— indicators of the scale of audiometry after absorption of carbon dioxide by burning copper chips, %;
— coefficient of correction for temperature and pressure (tabular value);
— the weight of the portion of alloy,
3.5.2. Discrepancies in the results of three parallel measurements (rate of convergence) and the results of the two tests
(index of reproducibility) shall not exceed the values of permissible differences given in the table.
3.5.3. Control of accuracy of analysis results is guaranteed by the establishing of operating mode according to the State standard samples (n.3.2) approved by GOST 8.315, in accordance with GOST 25086.
4. METHOD FOR THE DETERMINATION OF CARBON WITH THE USE OF AUTOMATIC AND SEMI-AUTOMATIC ANALYZERS
4.1. The essence of the method
The method is based on determining carbon analyser, providing the burning of the sample the sample of the alloy in a current of oxygen at 1300−1800 °C in the presence of flux. Mass fraction of carbon in percent is determined by the amount of the formed carbon dioxide a measurement of the amount of its absorbed infrared rays (IR spectroscopy) or the absorption of the formed carbon dioxide alkaline solution and determining the carbon (depending on the type of analyser) coulometric, conductometric or amperometric methods.
4.2. Equipment, reagents
The analyzer of any type, equipped with stove (induction, tubular or other type) for the combustion of samples in flowing oxygen with the detector operating on the principle of IR spectroscopy or other of the above principles.
Crucibles refractory ceramic for NTD, pre-calcined in a muffle furnace at a temperature of 1000−1100 °C for 3−4 h, stored in desiccator. Socket cover of the desiccator is not recommended to cover the lubricant. The shape and size of crucible chosen depending on the type of an applied device.
The beach:
the copper oxide in the form of wire or powder, is calcined at a temperature of (800±20) °C for 3−4 h;
the lead metal on the other 6−09−3523. A mixture of tin metal on the other 6−09−2705 and iron carbonising OSU 13−2 on the other 6−09−3000, taken in the ratio 2:1;
a mixture of tungsten metal SVC on the other 48−19−57 and tin metal on the other 6−09−2705, taken in the ratio 1:1.
Allowed the use of other flooded areas.
The ethyl ether acetic acid according to GOST 22300 or technical ethyl alcohol according to GOST 18300.
Oxygen technical GOST 5583 from coloradobased or oxygen.
Standard samples of Nickel alloys or carbon steels 2146−81 GSO, GSO 1862−80, GSO 1498−83п, GSO 1862−85п of the bonds 1609−85п of the bonds 888−84п, 1785−80 GSO, GSO 1774−84п of the bonds 1557−83п of the bonds 1640−83п.
4.3. Analysis
4.3.1. The device lead in working condition in accordance with the instructions.
A sample of alloy weighing 1 g, if necessary, washed with ether or alcohol, is placed in a ceramic crucible, cover linkage flux in the ratio 1:2 and carry out the analysis according to the instruction manual of the analyzer. The result of analysis is received on the basis of the readings or precise, given the values of the reference experiment.
In a control experiment carried out analysis of the prepared crucible with the addition of the applied flux.
4.3.2. The calibration of the analyzer is carried out on standard samples of steel type carbon or Nickel alloys. The results of the analysis are used for adjusting the settings of the analyzer.
Of the values of indications of the analyzer is subtracted value of the reference experience, according to the obtained values and corresponding carbon content in the standard samples to build a calibration curve or calculate the calibration function.
4.4. Processing of the results
4.4.1. Mass fraction of carbon in percent is calculated by the formula
where is the mass of carbon found on the calibration chart;
— the weight of the portion of the sample,
Note. The fully automated analysis on the digital display directly indicates the result of the analysis.
4.4.2. Discrepancies in the results of three parallel measurements (rate of convergence) and the results of the two tests
(index of reproducibility) shall not exceed the values allowable differences specified in table.1.
4.4.3. The control accuracy of the analysis was guaranteed by calibration of an analyzer according to the State standard samples (section 4.2) approved by GOST 8.315, in accordance with GOST 25086.
