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GOST 21639.1-90

GOST R ISO 15353-2014 GOST P 55080-2012 GOST R ISO 16962-2012 GOST R ISO 10153-2011 GOST R ISO 10280-2010 GOST R ISO 4940-2010 GOST R ISO 4943-2010 GOST R ISO 14284-2009 GOST R ISO 9686-2009 GOST R ISO 13899-2-2009 GOST 18895-97 GOST 12361-2002 GOST 12359-99 GOST 12358-2002 GOST 12351-2003 GOST 12345-2001 GOST 12344-88 GOST 12350-78 GOST 12354-81 GOST 12346-78 GOST 12353-78 GOST 12348-78 GOST 12363-79 GOST 12360-82 GOST 17051-82 GOST 12349-83 GOST 12357-84 GOST 12365-84 GOST 12364-84 STATE STANDARD P 51576-2000 GOST 29117-91 GOST 12347-77 GOST 12355-78 GOST 12362-79 GOST 12352-81 GOST P 50424-92 STATE STANDARD P 51056-97 GOST P 51927-2002 GOST P 51928-2002 GOST 12356-81 GOST R ISO 13898-1-2006 GOST R ISO 13898-3-2007 GOST R ISO 13898-4-2007 GOST R ISO 13898-2-2006 STATE STANDARD P 52521-2006 GOST P 52519-2006 GOST R 52520-2006 GOST P 52518-2006 GOST 1429.14-2004 GOST 24903-81 GOST 22662-77 GOST 6012-2011 GOST 25283-93 GOST 18318-94 GOST 29006-91 GOST 16412.4-91 GOST 16412.7-91 GOST 25280-90 GOST 2171-90 GOST 23401-90 GOST 30642-99 GOST 25698-98 GOST 30550-98 GOST 18898-89 GOST 26849-86 GOST 26876-86 GOST 26239.5-84 GOST 26239.7-84 GOST 26239.3-84 GOST 25599.4-83 GOST 12226-80 GOST 23402-78 GOST 1429.9-77 GOST 1429.3-77 GOST 1429.5-77 GOST 19014.3-73 GOST 19014.1-73 GOST 17235-71 GOST 16412.5-91 GOST 29012-91 GOST 26528-98 GOST 18897-98 GOST 26529-85 GOST 26614-85 GOST 26239.2-84 GOST 26239.0-84 GOST 26239.8-84 GOST 25947-83 GOST 25599.3-83 GOST 22864-83 GOST 25599.1-83 GOST 25849-83 GOST 25281-82 GOST 22397-77 GOST 1429.11-77 GOST 1429.1-77 GOST 1429.13-77 GOST 1429.7-77 GOST 1429.0-77 GOST 20018-74 GOST 18317-94 STATE STANDARD P 52950-2008 GOST P 52951-2008 GOST 32597-2013 GOST P 56307-2014 GOST 33731-2016 GOST 3845-2017 STATE STANDARD P ISO 17640-2016 GOST 33368-2015 GOST 10692-2015 GOST P 55934-2013 GOST P 55435-2013 STATE STANDARD P 54907-2012 GOST 3845-75 GOST 11706-78 GOST 12501-67 GOST 8695-75 GOST 17410-78 GOST 19040-81 GOST 27450-87 GOST 28800-90 GOST 3728-78 GOST 30432-96 GOST 8694-75 GOST R ISO 10543-99 GOST R ISO 10124-99 GOST R ISO 10332-99 GOST 10692-80 GOST R ISO 17637-2014 GOST P 56143-2014 GOST R ISO 16918-1-2013 GOST R ISO 14250-2013 GOST P 55724-2013 GOST R ISO 22826-2012 GOST P 55143-2012 GOST P 55142-2012 GOST R ISO 17642-2-2012 GOST R ISO 17641-2-2012 GOST P 54566-2011 GOST 26877-2008 GOST R ISO 17641-1-2011 GOST R ISO 9016-2011 GOST R ISO 17642-1-2011 STATE STANDARD P 54790-2011 GOST P 54569-2011 GOST P 54570-2011 STATE STANDARD P 54153-2010 GOST R ISO 5178-2010 GOST R ISO 15792-2-2010 GOST R ISO 15792-3-2010 GOST P 53845-2010 GOST R ISO 4967-2009 GOST 6032-89 GOST 6032-2003 GOST 7566-94 GOST 27809-95 GOST 22974.9-96 GOST 22974.8-96 GOST 22974.7-96 GOST 22974.6-96 GOST 22974.5-96 GOST 22974.4-96 GOST 22974.3-96 GOST 22974.2-96 GOST 22974.1-96 GOST 22974.13-96 GOST 22974.12-96 GOST 22974.11-96 GOST 22974.10-96 GOST 22974.0-96 GOST 21639.9-93 GOST 21639.8-93 GOST 21639.7-93 GOST 21639.6-93 GOST 21639.5-93 GOST 21639.4-93 GOST 21639.3-93 GOST 21639.2-93 GOST 21639.0-93 GOST 12502-67 GOST 11878-66 GOST 1763-68 GOST 13585-68 GOST 16971-71 GOST 21639.10-76 GOST 2604.1-77 GOST 11930.7-79 GOST 23870-79 GOST 11930.12-79 GOST 24167-80 GOST 25536-82 GOST 22536.2-87 GOST 22536.11-87 GOST 22536.6-88 GOST 22536.10-88 GOST 17745-90 GOST 26877-91 GOST 8233-56 GOST 1778-70 GOST 10243-75 GOST 20487-75 GOST 12503-75 GOST 21548-76 GOST 21639.11-76 GOST 2604.8-77 GOST 23055-78 GOST 23046-78 GOST 11930.11-79 GOST 11930.1-79 GOST 11930.10-79 GOST 24715-81 GOST 5639-82 GOST 25225-82 GOST 2604.11-85 GOST 2604.4-87 GOST 22536.5-87 GOST 22536.7-88 GOST 6130-71 GOST 23240-78 GOST 3242-79 GOST 11930.3-79 GOST 11930.5-79 GOST 11930.9-79 GOST 11930.2-79 GOST 11930.0-79 GOST 23904-79 GOST 11930.6-79 GOST 7565-81 GOST 7122-81 GOST 2604.3-83 GOST 2604.5-84 GOST 26389-84 GOST 2604.7-84 GOST 28830-90 GOST 21639.1-90 GOST 5640-68 GOST 5657-69 GOST 20485-75 GOST 21549-76 GOST 21547-76 GOST 2604.6-77 GOST 22838-77 GOST 2604.10-77 GOST 11930.4-79 GOST 11930.8-79 GOST 2604.9-83 GOST 26388-84 GOST 14782-86 GOST 2604.2-86 GOST 21639.12-87 GOST 22536.8-87 GOST 22536.0-87 GOST 22536.3-88 GOST 22536.12-88 GOST 22536.9-88 GOST 22536.14-88 GOST 22536.4-88 GOST 22974.14-90 GOST 23338-91 GOST 2604.13-82 GOST 2604.14-82 GOST 22536.1-88 GOST 28277-89 GOST 16773-2003 GOST 7512-82 GOST 6996-66 GOST 12635-67 GOST 12637-67 GOST 12636-67 GOST 24648-90

GOST 21639.1−90 Fluxes for electroslag remelting. Methods for determination of moisture content


GOST 21639.1−90

Group B09


STATE STANDARD OF THE USSR

FLUXES FOR ELECTROSLAG REMELTING

Methods for determination of moisture content

Fluxes for electroslag remelting.
Methods for determination of moisture content



AXTU 0809

Valid from 01.07.92
before 01.07.97*
_______________________________
* Expiration removed by Protocol No. 7−95
The interstate Council for standardization,
Metrology and certification (I & C N 11, 1995). -
Note the manufacturer’s database.



INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of heavy machine building of the USSR

DEVELOPERS

P. L. Babushkin, V. Y. Persits, PhD. chem. Sciences; Y. A. Margolin; M. P. Gerashchenko, V. A. of the chair (supervisor); Zelenova, O. B.; O. A. Raspopin; N. D. Vishniac

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on management of quality and standards from 29.12.90 N 3472

3. REPLACE GOST 21639.1−76

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
Item number
GOST 4204−77
3.2
GOST 4328−77
3.2
GOST 5583−78
3.2
GOST 9147−80
3.3
GOST 21639.0−76
Sec. 1
GOST 24104−88
3.2
GOST 25336−82
2.2, 3.2
THAT 6−09−3880−75
3.2
THAT 6−09−4010−75
3.2
THAT 6−09−5382−88
3.2



This standard specifies gravimetric methods for determination of hygroscopic moisture in the mass fraction of from 0.5 to 5.0% and total moisture for the mass concentration of from 0.01 to 5.0% in fluxes for electroslag remelting.

1. GENERAL REQUIREMENTS


General requirements for methods of analysis GOST 21639.0*.
_______________
* Valid GOST 21639.0−93. — Note the manufacturer’s database.

2. METHOD OF DETERMINATION OF HYGROSCOPIC MOISTURE

2.1. The essence of the method

The method is based on drying of the sample flux at a temperature of 105−110 °C to constant weight.

2.2. Equipment

Analytical scale with weights.

Drying oven electrically heated and thermostat.

Cups for weighing (buxy) according to GOST 25336.

Desiccator, according to GOST 25336 filled with calcium chloride for NTD.

2.3. Analysis

A portion of the flux weight of 20−50 g was placed in buxu, pre-dried at 105−110 °C to constant weight and weighed with lid.

Then bucsu a hitch and the cover removed is dried in a drying Cabinet at 105−110 °C for 2 h, covered with a lid, cooled in a desiccator and weighed 30−40 minutes.

Before weighing cover buxy slightly open to equalize the pressure and quickly closed. Repeat drying for 30 minutes to constant weight. If re-weighting is an increase in mass, the final result of taking a lot prior to its increase.

2.4. Processing of the results

2.4.1. Mass fraction of hygroscopic moisture (ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги) in percent is calculated by the formula

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги,

where ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влагиis the mass of buxy with the suspension before drying, g;

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги — weight boxy a hitch after drying, g;

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги — the weight of the portion,

2.4.2. Allowable absolute differences of the results of the parallel definitions should not exceed the values given in table.1.

Table 1

   
Mass fraction of hygroscopic moisture, %
Allowable absolute differences, %
From 0.05 to 1.00 incl.
0,05
SV. 1,00 «2,00 «
0,10
«2,00» 4,00 «
0,20
«4,00» 5,00 «
0,30

3. METHOD FOR THE DETERMINATION OF TOTAL MOISTURE

3.1. The essence of the method

The method is based on heating of the analyte in a tube furnace at a temperature of 1000 °C in flowing oxygen, turning the contained hydrogen in the moisture and its gravimetric determination after absorption of magnesium perchlorate (angerona). To reduce the error of analysis of the evolved gaseous compounds of fluorine are absorbed by the lead monoxide at the exit of the tube.

3.2. Apparatus, reagents and solutions

Setup for determination of moisture (Fig.1) consists of the oxygen cylinder (1) according to GOST 5583, equipped with a pressure reducing valve start-up and adjustment of a current of oxygen; reducer pressure gauge (2) — fine adjustment of oxygen; safety bulb (3), which in case of overpressure in the combustion chamber prevents the ingress of sulfuric acid in the rubber tubing connecting the device with a reducing valve; the system of cleaning and drying of oxygen, rinsing the flask (4) with sulfuric acid; drying columns (5) and (6), filled with granulated sodium hydroxide and magnesium perchlorate; a porcelain tube (7) length of 500 mm and an inner diameter of 20−25 mm; tube furnaces (8) brand SUOL-0.25.1/12-M1; asbestos tube (9), saturated with lead monoxide, heated to a temperature of 800 °C. copper tube (10) heated to a temperature of 110−120 °C; an l-shaped pipe (11); the absorption flasks (12) with magnesium perchlorate (angerona). L-shaped pipeline made of austenitic stainless steel and consists of two symmetrical separable parts, the total length of the pipeline is 750 mm. the Spiral heater is placed around and along the curved profile of the pipeline copper pipe while also isolating the heater turns of asbestos cord CHAON-3 impregnated with liquid glass. A tube with a heater braid tape made of PTFE and placed in the lower part of the housing pipeline, pre-lined with kaolin wool, top up with the heater also cover the kaolin wool and covers the upper part of the housing pipeline. Both parts of the case fasten with screws through the holes in the ears welded to the upper and lower parts of the pipeline.

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги


Damn.1



Permitted heaters and absorption flasks other structures providing the required accuracy of the analysis.

The hook with which the boat was placed in a tube and extracted from it, is made of heat-resistant wire with a diameter of 3−5 mm and a length of 400−600 mm.

To install the tube in a porcelain tube using a special pusher with the catch.

Laboratory scales for General purpose according to GOST 24104*, not lower than 2nd accuracy class with the largest weighing limit of 200 g or other scales that meets the specified requirements for their metrological characteristics.
_______________
* On the territory of the Russian Federation GOST 24104−2001, here and hereafter. — Note the manufacturer’s database.


To determine the mass fraction from 0.01 to 0.03% use laboratory scales for General purpose according to GOST 24104 is not below 1st class of accuracy.

Sulfuric acid according to GOST 4204.

Sodium hydroxide according to GOST 4328.

Of magnesium perchlorate on the other 6−09−3880.

Kaolin wool or asbestos fiber on the other 6−09−4010.

Lead monoxide (II) on the other 6−09−5382.

3.3. Preparation for assay

Pour in the rinse flask (4) 125 cmГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влагиof sulfuric acid. Drying columns (5) and (6), and the absorption flask (12) is prepared to work in accordance with the devil.2. The mass absorption flasks prepared in the form of (70±2) g. of magnesium Perchlorate should not asiatica tightly. Absorption flask with a diameter of 30 mm in the lower part 5−6 holes with a diameter of (1±0,2) mm Height of the absorption bulb 105 mm.

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги


1 — glass wool; 2 — absorber; 3 — glass wool

Damn.2



In calcined along the entire length of the porcelain tube is placed a tube, impregnated with lead monoxide. Tube (9) from long-fibre asbestos or kaolin wool, pre-calcined at 400 °C for 30 min, prepared as follows: a steel brush pour a uniform layer of fibrous asbestos or kaolin wool and evenly cover the asbestos co-lead. By rubbing two steel brushes provide uniform distribution of monoxide lead asbestos. The excess of lead monoxide shake sieve. For impregnation of 100 g of asbestos requires about 100 g of monoxide of lead. 4,5−5,0 g impregnated asbestos (kaolin wool) is sufficient for the formation of the tube. Both sides of the tube are placed glass wool 10 mm on each side (Fig.3).

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги


Damn.3



The constancy of oxygen consumption is determined by the rotameter (2), which is installed in front of the safety bulb. The flow of oxygen through the system occurs at a rate of 175−225 cmГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги/min.

Before starting, heat the oven to a temperature of 1000 °C and check the installation for leaks. For this connect instead of the absorption of the bulb (12) glass tube, the end of which dipped into a Cup of water and interrupt the flow of oxygen, holding the hose in front of the safety bulb. If the water in the glass tube rises, the system is sealed.

The ends of helical heater located around and along the curved profile of the pipeline (11) copper tubes (10), connected to latro RNO-250−2 and set the voltage to the outlet temperature of the copper tube was 110−120 °C.

Porcelain boats N 2 — according to GOST 9147 or quartz boat (length of 100−120 mm, width 15−20 mm, height 10 mm) was calcined in flowing oxygen at a temperature of 1000 °C before operation.

Before starting, set the average value of the blank experience. After the furnace temperature reaches 1000 °C flow and oxygen consumption 175−225 cmГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги/min, weighing of the absorption flask (12) every 5−7 min. Installation ready to use when the difference in weight between each weighing not more than 0.2−0.4 mg. the Value of the idle experience more than 0.4 mg demonstrates the need for prevention of the installation.

To do this, you must replace the reagents used for the dehydration of oxygen (sulfuric acid, sodium hydroxide and magnesium perchlorate) and to clean from contamination all parts of the installation.

Tube (9) provides a delay of fluorides for the total number of tests. Control over the operation of the tube is carried out by changing the color of perchlorate of magnesium in the absorption flask (12), caused by penetration of fluoride.

3.4. Analysis

Weighed samples of ground mounted depending on the mass fraction of moisture on the table.2, placed in a porcelain or quartz boat.

Table 2

   
Mass fraction of moisture, %
The weight of the portion of flux, g
From 0,01 to 0,03 incl.
7−10
SV. Of 0.03 «to 0.07 «
4 — 7
«To 0.07» to 0.20"
2−4
«To 0.20» to 1.00 «
0,5−2,0
«To 1.00» 5,00 «
1,0−0,1



A boat with a hook is introduced into the most heated portion of the porcelain tube (7) and tightly closed the tube with a rubber stopper through which passed a tube to supply oxygen. The moisture extracted from the sample is distilled in an absorption flask (12), while volatile side-products and fluoride are absorbed by the lead monoxide at the exit of the tube. The sample left in the furnace until, while in the upper part of the glass tube and absorption of the bulb (12) there will be condensation (no more than 5−7 minutes). Then seal the absorption flask (12), closing the upper hole tube and the lower hole for the output of the oxygen tight rubber ring and weighed. Remove analyzed sample from the oven, connect the absorption flask (12) to install and start analyzing the next sample.

3.5. Processing of the results

3.5.1. Mass fraction of moisture (ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги) in percent is calculated by the formula

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги,


where ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влагиis the mass absorption flasks after analysis, g;

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги — the mass of the same flask prior to analysis, g;

ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги — the weight of the portion of the flux to be analyzed,

3.5.2. Allowable absolute differences of the results of three parallel measurements at a confidence level ГОСТ 21639.1-90 Флюсы для электрошлакового переплава. Методы определения содержания влаги=0.95 does not exceed the values given in table.3.

Table 3

   
Mass fraction of moisture, %
Allowable absolute differences, %
From 0.01 to 0.02 incl.
0,004
SV. 0,02 «0,05 «
0,008
«0,05» 0,10 «
0,010
«To 0.10» to 0.30 «
0,030
«0,30» to 1.00 «
0,050
«1,00» 2,00 «
0,100
«2,00» 5,00 «
0,200