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Tiêu đề Part 2: Methods of test
Trường học Unknown University
Chuyên ngành Electrical Engineering
Thể loại Standards document
Năm xuất bản 2001
Thành phố Unknown
Định dạng
Số trang 78
Dung lượng 1,03 MB

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Cấu trúc

  • 5.1 Détermination de l'épaisseur des feuilles de papier unitaires (ISO 534) (18)
  • 5.2 Détermination de l'épaisseur moyenne du papier (18)
  • 10.1 Appareil d'essai (22)
  • 10.2 Eprouvettes (22)
  • 10.3 Mode opératoire (22)
  • 10.4 Résultats (24)
  • 12.1 Appareil d'essai (24)
  • 12.2 Eprouvettes (24)
  • 12.3 Mode opératoire (24)
  • 12.4 Résultats (24)
  • 15.1 Appareil d'essai (26)
  • 15.2 Mode opératoire (26)
  • 15.3 Résultats (28)
  • 16.1 Appareil d'essai (28)
  • 16.2 Mode opératoire (28)
  • 16.3 Résultats (28)
  • 17.1 Méthode 1 (30)
  • 17.2 Méthode 2 (32)
  • 5.1 Determination of the thickness of single sheets of paper (ISO 534) (19)
  • 5.2 Determination of mean thickness of paper (19)
  • 10.1 Test apparatus (23)
  • 10.2 Test pieces (23)
  • 10.3 Procedure (23)
  • 10.4 Results (25)
  • 12.1 Test apparatus (25)
  • 12.2 Test pieces (25)
  • 12.3 Procedure (25)
  • 12.4 Results (25)
  • 15.1 Test apparatus (27)
  • 15.2 Procedure (27)
  • 15.3 Results (29)
  • 16.1 Test apparatus (29)
  • 16.2 Procedure (29)
  • 16.3 Results (29)
  • 17.1 Method 1 (31)
  • 17.2 Method 2 (33)
  • 19.1 Appareil d'essai (34)
  • 19.2 Mode opératoire (36)
  • 19.3 Résultats (36)
  • 21.1 Appareil d'essai (38)
  • 21.2 Eprouvettes (40)
  • 21.3 Mode opératoire (40)
  • 21.4 Résultats (40)
  • 22.1 Principe (40)
  • 22.2 Réactif (40)
  • 22.3 Appareillage (40)
  • 22.4 Conditionnement (42)
  • 22.5 Eprouvettes (42)
  • 22.6 Procédure (42)
  • 22.7 Résultats (44)
  • 22.8 Rapport d'essai (44)
  • 23.1 Appareil d'essai (44)
  • 23.2 Eprouvettes (46)
  • 23.3 Mode opératoire (46)
  • 23.4 Résultats (46)
  • 24.1 Appareil d'essai (48)
  • 24.2 Eprouvettes (48)
  • 24.3 Mode opératoire (48)
  • 24.4 Résultats (48)
  • 24.5 Méthode d'essai utilisant une tension continue (48)
  • 25.1 Appareil d'essai (52)
  • 25.2 Eprouvettes (54)
  • 25.3 Mode opératoire (54)
  • 25.4 Résultats (56)
  • 26.1 Méthode 1 (56)
  • 26.2 Méthode 2 (58)
  • 27.1 Résistance interne au déchirement (62)
  • 27.2 Résistance à l'éclatement (62)
  • 27.3 Degré de polymérisation (62)
  • 19.1 Test apparatus (35)
  • 19.2 Procedure (37)
  • 19.3 Results (37)
  • 21.1 Test apparatus (39)
  • 21.2 Test pieces (41)
  • 21.3 Procedure (41)
  • 21.4 Results (41)
  • 22.1 Principle (41)
  • 22.2 Reagent (41)
  • 22.3 Apparatus (41)
  • 22.4 Conditioning (43)
  • 22.5 Test pieces (43)
  • 22.6 Procedure (43)
  • 22.7 Results (45)
  • 22.8 Test report (45)
  • 23.1 Test apparatus (45)
  • 23.2 Test pieces (47)
  • 23.3 Procedure (47)
  • 23.4 Results (47)
  • 24.1 Test apparatus (49)
  • 24.2 Test pieces (49)
  • 24.3 Procedure (49)
  • 24.4 Results (49)
  • 24.5 Test method using d.c. voltage (49)
  • 25.1 Test apparatus (53)
  • 25.2 Test pieces (55)
  • 25.3 Procedure (55)
  • 25.4 Results (57)
  • 26.1 Method 1 (57)
  • 26.2 Method 2 (59)
  • 27.1 Internal tearing resistance (63)
  • 27.2 Bursting strength (63)
  • 27.3 Degree of polymerization (63)

Nội dung

Cette éprouvette peut être prélevée sur un échantillon ou, dans certains cas, être l'échantillon lui-même 4 Remarques générales sur les essais Sauf spécification contraire, l'échantillon

Détermination de l'épaisseur des feuilles de papier unitaires (ISO 534)

La méthode repose sur l'emploi d'un micromètre de précision à cadran pour la mesure de l'épaisseur d'une feuille unitaire sous charge statique.

La charge statique à appliquer doit correspondre à une pression de 100 kPa ± 10 kPa. b) Exceptions

The test must be conducted on three conditioned specimens Each of the three specimens undergoes a determination, which involves taking five measurements at the four corners and the center of the specimen.

Les résultats sont exprimés en micromètres.

Lorsque des mesures sont effectuées sur toute la largeur pour établir la variation transversale d'épaisseur, les détails de ce mode opératoire seront indiqués dans la CEI 60554-3.

Détermination de l'épaisseur moyenne du papier

La méthode repose sur l'emploi d'un micromètre de précision à cadran pour la mesure d'un empilage composé de cinq feuilles au moins.

La charge statique à appliquer doit correspondre à une pression de 100 kPa ± 10 kPa.

The test must be conducted on three conditioned specimens, each consisting of at least five sheets measuring 250 mm × 250 mm, taken from the same sample A determination is made for each of the three specimens, which involves five measurements taken at the four corners and the center of the specimen.

For narrow materials with a width less than the mandated 250 mm, five measurements must be taken at approximately equal intervals on a 400 mm long specimen.

Les résultats sont exprimés en micromètres pour l'épaisseur d'une feuille unitaire.

Lorsque des mesures sont effectuées sur toute la largeur pour établir la variation transversale d'épaisseur, les détails de ce mode opératoire seront indiqués dans la CEI 60554-3.

6 Grammage du papier (masse par mètre carré, poids de base ou substance)

Le grammage doit être mesuré selon la méthode décrite dans l'ISO 536, avec les exceptions suivantes:

– il n'est pas tenu compte des articles 5 et 6 de l'ISO 536;

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Thickness shall be measured in accordance with ISO 534 with the exceptions given below.

5.1 Determination of the thickness of single sheets of paper (ISO 534) a) Principle

The method is based on the use of a precision dial micrometer to measure the thickness of a single sheet when a static load is applied.

The static load to be applied shall correspond to a pressure of 100 kPa ± 10 kPa. b) Exceptions

The test will be conducted on three conditioned test pieces, with one determination performed on each piece Each determination includes five measurements: one at each corner and one in the center of the test piece.

The results are given in microns.

Where thickness is determined across the width to establish the variation over the width, the details of this procedure will be found in IEC 60554-3.

5.2 Determination of mean thickness of paper

The method is based on the use of a precision dial micrometer to measure the thickness of a stack composed of a minimum of five sheets.

The static load to be applied shall correspond to a pressure of 100 kPa ± 10 kPa.

The test will be conducted on three conditioned samples, each made up of at least five sheets measuring 250 mm × 250 mm from a single specimen Each of the three samples will undergo one determination, which includes five measurements taken at each corner and one in the center of the test piece.

For narrow material where the width is less than the stipulated 250 mm, the five measurements on each stack shall be made at approximately equal intervals on a specimen measuring

The results are given in terms of the thickness of a single sheet in microns.

Where thickness is determined across the width to establish the variation over the width, the details of this procedure will be found in IEC 60554-3.

6 Substance (mass per square metre, basic weight or grammage)

Paper grammage shall be measured according to the method described in ISO 536 with the following exceptions:

– clauses 5 and 6 of ISO 536 are ignored;

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– l'essai doit être effectué sur trois éprouvettes conditionnées, une détermination étant faite sur chacune des trois éprouvettes;

– la masse doit être déterminée, à 0,5 % près, sur des éprouvettes conditionnées d'au moins

The surface area and mass of each specimen are measured, and the unit mass is calculated in grams per square meter, with all measurements taken on conditioned specimens.

Lorsque des mesures sont effectuées sur toute la largeur pour établir la variation transversale du grammage, les détails de ce mode opératoire seront indiqués dans la CEI 60554-3.

The thickness and grammage are determined for each of the three samples as outlined in Articles 5 and 6 For each sample, the apparent density is calculated, which is expressed in grams per cubic centimeter.

8 Résistance à la traction et allongement

La résistance à la traction et l'allongement doivent être mesurés conformément à l’une des méthodes décrites dans l'ISO 1924, avec les exceptions suivantes (la méthode à utiliser doit être indiquée dans la CEI 60554-3):

– des mesures sont effectuées sur neufs éprouvettes coupées dans le sens machine et sur neuf autres coupées dans le sens transversal;

– la valeur médiane des mesures, dans chaque sens, est prise comme résultat; les valeurs maximale et minimale dans chaque sens sont consignées;

– les résultats pourront éventuellement être exprimés sous forme de longueur de rupture, en mètres, arrondis à la tranche de 100 m la plus proche.

The measurement of the tensile force required to break 15 mm specimens, approximately 250 mm in length, cut in both directions of the paper, is conducted under standardized testing conditions.

The internal tear resistance must be measured according to the testing method outlined in ISO 1974 A simple tear resistance measuring device should be utilized, with the following exceptions.

– des mesures sont effectuées sur neuf éprouvettes coupées dans le sens machine et sur neuf autres dans le sens transversal.

Eprouvettes rectangulaires comportant une seule entaille, laissant une longueur de 43 mm à déchirer Mesure de l'énergie requise pour déchirer ces 43 mm.

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– the test shall be carried out on three conditioned test pieces, one determination being made on each of the three test pieces;

– the mass is to be determined to an accuracy of 0,5 % on conditioned test pieces of not less than 500 cm 2

The mass and area of each conditioned test piece are measured, allowing for the calculation of mass per unit area in grams per square meter.

Where grammage is determined across the width to establish the variation over the width, the details of this procedure will be found in IEC 60554-3.

The thickness and grammage of each of the three test pieces are measured according to clauses 5 and 6 Additionally, the apparent density is calculated for each test piece, which is expressed in grams per cubic centimeter.

Tensile strength and elongation shall be measured according to one of the methods described in ISO 1924 with the following exceptions (the method to be used shall be indicated in

– measurements are made on nine test pieces cut from the machine direction and on nine others cut from the cross direction;

– the central value of the measurements, in each direction, is taken as the result and the highest and the lowest values in each direction are reported;

– alternatively, the results can be expressed as the breaking length in metres rounded to the nearest 100 m.

Measurement of the tensile force required to cause failure of test pieces 15 mm by approximately 250 mm, cut from both directions of the paper, when applied under standard test conditions.

Internal tearing resistance shall be measured according to the method described in ISO 1974.

The single-tear tester shall be used with the following exceptions:

– measurements are made on nine test pieces cut from the machine direction and nine others from the cross direction.

Rectangular test pieces having a single cut leaving 43 mm length to be torn Measurement of the energy required to tear this.

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10 Résistance au déchirement des bords

Appareil d'essai

A tear strip clamp (see Figure 1) must be used, which is attached to the tensile testing device as outlined in ISO 1924 The tear strip clamp consists of a thin steel plate (A) that serves as a vertical support, with its edge resting on the ends of a forked frame.

The thin metallic silk of the stirrup frame is secured in the lower jaw of the tensile testing machine, ensuring that the vertical midline of the stirrup aligns with the imaginary line connecting the central points of the upper and lower jaws The vertical plate can be removed from the stirrup frame, and two plates of different thicknesses are provided for testing papers of varying thicknesses One plate has a thickness of 1.25 mm ± 0.05 mm, while the other measures 2.50 mm ± 0.05 mm.

The edge of the plate features a shallow V-shaped notch, with sides forming an angle of approximately 150° ± 1° The V-notch sides have a semi-circular cross-section and must be perfectly smooth and straight.

Eprouvettes

Nine test specimens should be cut in the machine direction and nine others in the cross direction of the paper; they must be between 15 mm and 25 mm wide and at least 250 mm long.

Les éprouvettes doivent être conditionnées conformément à l'article 4.

Mode opératoire

Fixer une plaque d'épaisseur convenable sur le bâti de l'étrier On montera la plaque de 1,25 mm ± 0,05 mm pour les papiers de 0,75 mm d'épaisseur maximale, et la plaque de

2,50 mm ± 0,05 mm pour les papiers plus épais.

Secure the thin silk of the stirrup in the lower jaw of the tensile testing device, ensuring that the vertical midline of the stirrup aligns with the imaginary line connecting the central points of the upper and lower jaws Additionally, position the sides of the V-notch symmetrically relative to the line that runs through these central points.

NOTE Si nécessaire, l'étrier pourra être fixé dans la mâchoire supérieure Dans ce cas, l'appareil d'essai de résistance à la traction sera rééquilibré pour compenser la masse de l'étrier.

Position the lower jaw of the device so that the lower edge of the upper jaw is approximately 90 mm above the upper edge of the plate featuring the V-notch.

Enfiler l'éprouvette dans l'étrier, sous la plaque, et réunir les deux extrémités en les fixant dans la mâchoire supérieure.

This operation will effectively reduce most of the slack in the specimen; however, care must be taken to avoid applying a tearing force Whenever possible, the initial increases in the load applied to the specimen should be done very gently to prevent abnormal stresses caused by inertia effects.

Augmenter la charge pour que le déchirement se produise entre 5 s et 15 s; consigner cette charge, exprimée en newtons.

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An edge-tear stirrup, as illustrated in figure 1, must be utilized and connected to the tensile testing apparatus in accordance with ISO 1924 standards This stirrup features a thin steel plate (A) that acts as a vertical plate, supported at the edge by the ends of a stirrup-shaped frame.

The stirrup frame's thin metal tang is secured in the lower clamp of the tension testing machine, aligning its vertical center line with the midpoint connection of the upper and lower clamps A removable vertical plate is included with the stirrup frame, accompanied by two plates of varying thicknesses for different paper thickness ranges: one measuring 1.25 mm ± 0.05 mm and the other 2.50 mm ± 0.05 mm Each plate features a shallow V-notch with sides that form a 150° ± 1° angle, and the V-notch sides are designed to be smooth and straight with a semicircular cross-section.

A total of eighteen test pieces will be prepared, with nine cut in the machine direction and nine in the cross direction of the paper Each piece will measure between 15 mm and 25 mm in width and will have a minimum length of 250 mm.

The test pieces shall be conditioned according to clause 4.

Attach a plate of the proper thickness to the stirrup frame The plate with the thickness of

1,25 mm ± 0,05 mm is to be used for papers of up to 0,75 mm in thickness and the plate with the thickness of 2,50 mm ± 0,05 mm for thicker papers.

Secure the thin tang of the stirrup in the lower clamp of the tension-testing machine, ensuring that the vertical center line of the stirrup aligns with the line connecting the mid-points of the upper and lower clamps Additionally, position the sides of the V-notch symmetrically with respect to the line through the mid-points of the clamps.

NOTE The stirrup may be fastened in the upper clamp, if desired This procedure will require rebalancing the tension-testing machine to compensate for the mass of the stirrup.

Place the lower clamp of the machine so that the lower edge of the upper clamp is about

90 mm above the upper edge of the V-notched plate.

Thread the test piece through the stirrup, under the plate, and bring the two ends together and fasten them in the upper clamp.

During this operation, it is crucial to absorb most of the slack in the test piece without applying a tearing force To minimize abnormal strains caused by inertia effects, the initial increments of load should be applied to the test piece very slowly whenever possible.

Increase the load so that tearing starts in 5 s to 15 s and record this load in newtons.

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Résultats

Record the median values, expressed in newtons, for both directions of the paper, noting the thickness of the plate used, the load application speed, as well as the width and thickness of the specimens.

La résistance à l'éclatement doit être déterminée conformément à la méthode décrite dans l'ISO 2758, avec les exceptions suivantes:

– les éprouvettes doivent être conditionnées conformément à l'article 4.

A test tube is rigidly attached to the perimeter of a circular elastic diaphragm while remaining free to bulge with it A hydraulic fluid is pumped at a constant rate to inflate the diaphragm until the test tube breaks The burst strength of the test tube represents the maximum value of the applied hydraulic pressure.

Appareil d'essai

Un appareil d'essai de pliage (type Schopper).

Eprouvettes

Neuf bandes de 15 mm de large, découpées dans le sens machine, et neuf autres bandes découpées dans le sens transversal.

Mode opératoire

Clamp the test specimen between the two jaws Apply a tension of 5 N for specimens up to 0.03 mm thick, or 10 N for thicker specimens Determine the number of double folds the paper can withstand around a plate that is 0.5 mm thick with a curvature radius of 0.25 mm, at a speed of 100 to 200 double folds per minute.

Résultats

Consigner la valeur médiane de chaque série, jusqu'à deux chiffres significatifs, ainsi que les valeurs maximale et minimale.

The moisture content of paper upon receipt must be measured according to the method outlined in ISO 287 (oven drying method) The result should be expressed as a percentage of moisture relative to the initial mass Three samples should be taken in accordance with ISO 287.

Peser l'éprouvette au moment de l'échantillonnage et, la peser de nouveau, après dessiccation jusqu'à masse constante, dans une étuve portée à une température comprise entre 102 °C et

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The central values for both directions of the paper are reported in newtons, taking into account the plate thickness, loading rate, and the dimensions of the test pieces, including their width and thickness.

The bursting strength shall be determined according to the method described in ISO 2758, with the following exceptions:

– the test pieces shall be conditioned in accordance with clause 4.

A test specimen is securely clamped around its edges while being in contact with a circular elastic diaphragm, allowing it to bulge as the diaphragm expands Hydraulic fluid is continuously pumped at a steady rate, causing the diaphragm to inflate until the test specimen fails The maximum hydraulic pressure applied at the moment of rupture determines the bursting strength of the test specimen.

Nine strips 15 mm wide, cut in the machine direction, and nine other strips cut in the cross direction.

Clamp the specimen securely in both clamps and apply a tension of 5 N for specimens up to 0.03 mm thick, or 10 N for thicker specimens Measure the number of double folds the paper can endure by using a plate that is 0.5 mm thick with a curvature radius of 0.25 mm, at a speed of 100 to 200 double folds per minute.

Report the central value of each series to two significant figures The highest and lowest values shall also be reported.

The moisture content of the received paper must be measured using the oven-drying method outlined in ISO 287, with results reported as a percentage of the original mass Additionally, three test specimens should be collected in accordance with ISO 287.

Weigh the test piece at the time of sampling and again after drying in an oven at 102 °C to

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La quantité de résidu de papier subsistant après l'incinération doit être déterminée confor- mément à la méthode décrite dans l'ISO 2144.

Il doit être procédé à trois déterminations Le résultat doit être exprimé en pourcentage de la masse séchée à l'étuve.

Appareil d'essai

– Une cellule de mesure de la conductivité dont la constante K est connue.

A measuring device is capable of assessing conductance or inductance, with a minimum indication of 1 aS and an accuracy of 5%, across a frequency range of 50 Hz to 3000 Hz Additionally, resistance can be measured with the same level of precision.

– Des flacons coniques de 250 cm 3 , à large goulot, en verre résistant aux acides et aux alcalis, équipés de condenseurs à reflux.

Mode opératoire

The determination must be conducted on the material in its received state Three extractions should be performed, with each requiring a measurement A preliminary control test must be carried out using water that has been boiled for 60 minutes ± 5 minutes in the designated flask If the conductivity of this water does not exceed 200 µS/m, the flask may be used.

If the conductivity exceeds the specified value, it is necessary to boil a new quantity of water in the same flask Should the conductivity measured after the second test surpass 200 µS/m, a different flask must be used.

L'essai sur le papier doit être effectué comme suit.

Découper un échantillon, pesant environ 20 g, en morceaux d'environ 10 mm × 10 mm Peser

5 g de matière dans un flacon en verre de 250 cm 3 équipé d'un condenseur à reflux et ajouter

To ensure accurate results, 100 cm³ of water with a conductivity not exceeding 200 µS/m should be gently boiled for 60 minutes, with a tolerance of ± 5 minutes After boiling, allow the water to cool in the container to room temperature while taking precautions to prevent the absorption of carbon dioxide from the air.

The extract is then transferred to a measuring container for immediate conductivity determination The measuring container must be rinsed twice with the extract Conductivity measurements should be conducted at a temperature of 23°C ± 0.5 K.

NOTE 1 L'extraction selon la méthode 1 de l'article 17 peut être admise en variante, mais on utilisera alors 5 g dans 100 cm 3

During the collection, storage, and handling of samples and test tubes intended for conductivity, pH, and chloride content testing of aqueous extracts, it is crucial to prevent contamination from the atmosphere, particularly in a chemical laboratory, as well as from direct hand contact.

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The amount of residue of paper left after incineration shall be determined according to the method described in ISO 2144.

Three determinations shall be made The result shall be expressed as a percentage of the oven dry mass.

– A conductivity cell with known cell constant K.

– A conductance or inductance measuring instrument, capable of measuring conductance to a minimum reading of 1 àS with an accuracy of 5 %, in the frequency range 50 Hz to 3 000 Hz.

Alternatively, the resistance may be measured with the same accuracy.

– Wide-mouth 250 cm 3 conical flasks with reflux condensers in acid- and alkali-resistant glass.

The determination of material quality is based on the received sample A measurement will be conducted for each of the three extractions Initially, a blank test will be performed using water that has been boiled for approximately 60 minutes in the designated flask If the conductivity of this water is 200 µS/m or lower, the flask is deemed suitable for use However, if the conductivity exceeds this threshold, the flask must be reboiled with a new batch of water for further testing.

200 àS/m, then another flask shall be used.

The test on the paper shall then be carried out as follows.

Cut a test specimen weighing approximately 20 g into pieces of about 10 mm × 10 mm Weigh approximately 5 g into a 250 cm 3 glass flask with a reflux condenser and add approximately

To ensure accurate results, 100 cm³ of water with a conductivity not exceeding 200 µS/m should be gently boiled for 60 minutes, with a tolerance of ± 5 minutes, and then allowed to cool to room temperature in a flask It is essential to take precautions to prevent the absorption of carbon dioxide from the air during this process.

The extract is decanted into a measuring vessel for immediate conductivity measurement, which should be rinsed twice with the extract Conductivity measurements must be conducted at a temperature of 23 °C ± 0.5 K.

NOTE 1 Extraction in accordance with method 1 of clause 17 is an acceptable alternative, but 5 g in 100 cm 3 is to be used.

To prevent contamination during the collection, storage, and handling of specimens and test portions for conductivity, pH, and chloride content tests of aqueous extracts, it is crucial to avoid exposure to atmospheric pollutants, especially in a chemical laboratory, and to refrain from using bare hands during handling.

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Résultats

Calculer la conductivité de la solution extraite comme suit: γ = K (G 1 – G 2 ) ó γ est la conductivitộ de l'extrait, exprimộe en microsiemens par mốtre (àS/m);

K est la constante de la cellule, exprimée en m –1 ;

G 1 est la conductance de l'extrait, exprimộe en microsiemens (àS);

G 2 est la conductance du tộmoin, exprimộe en microsiemens (àS).

Appareil d'essai

– Un pH-mètre avec des électrodes en verre et en calomel ayant une sensibilité minimale de 0,05 unité pH.

– Des flacons coniques de 250 cm 3 , à large goulot, en verre résistant aux acides et aux alcalis.

Mode opératoire

Il doit être procédé à trois extractions dont chacune fera l'objet d'une mesure.

Préparer un extrait comme cela est décrit en 15.2.

The extract should only be transferred at the time of use to prevent unnecessary exposure to ambient air Calibrate the pH meter using a reference solution with a pH within ±2 units of the extract's pH After calibration, carefully rinse the electrodes in distilled water multiple times and once in a small amount of the extract.

Immerger les électrodes dans l'extrait non filtré et mesurer la valeur du pH de celui-ci à une température de 23 °C ± 2 K.

When using the extract to determine conductivity, it is essential to collect the sample from the aqueous extract prior to measuring the pH This is important because potassium chloride released by the calomel electrode could skew the results.

Résultats

Consigner la valeur médiane comme étant le résultat; les valeurs maximale et minimale sont consignées.

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Calculate the conductivity of the extract solution as follows: γ = K (G 1 – G 2 ) where γ is the conductivity of extract solution, expressed in microsiemens per metre (àS/m);

K is the cell constant, expressed in m –1 ;

G 1 is the conductance of the extract solution, expressed in microsiemens (àS);

G 2 is the conductance of the blank test, expressed in microsiemens (àS).

– A pH-meter with glass and calomel electrodes having a sensitivity of at least 0,05 pH units.

– Wide-mouth 250 cm 3 conical flasks in acid- and alkali-resistant glass.

One measurement shall be made on each of three extractions.

Prepare an extract as described in 15.2.

To ensure optimal results, decant the extract only for immediate use to minimize atmospheric exposure Calibrate the pH meter using a buffer solution with a pH value within ±2 units of the extract's pH After calibration, thoroughly rinse the electrodes in distilled water and then in a small amount of the extract.

Immerse the electrodes in the unfiltered extract and measure the pH value of the extract at

For accurate conductivity measurements, it is essential to collect the sample from the aqueous extract before determining the pH This is crucial because potassium chloride, which diffuses from the calomel electrode, can interfere with the results.

Report the central value as the result; the highest and lowest values are reported.

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17 Teneur en chlorure de l'extrait aqueux

Méthode 1

All equipment used in this experiment must be thoroughly clean It is recommended to boil all flasks, beakers, and funnels in deionized water after normal cleaning and rinsing The apparatus should be handled with stainless steel tongs Additionally, tweezers and scissors used for sample preparation should also be made of stainless steel and cleaned in the same manner.

NOTE Voir également note 2 de 15.2.

– Un appareil de mesure capable de mesurer une tension continue dans la gamme de 0 mV à

300 mV, avec une précision de 2 mV (par exemple un voltmètre électronique ou un potentiomètre tel qu'un pH-mètre).

– Un flacon en quartz ou en verre à haute résistance, à fond plat, d'une contenance de 600 cm 3

– Une seringue en verre à micromètre (pour la méthode 1 uniquement).

– Une microburette graduée en divisions de 0,01 cm 3 (pour la méthode 2 uniquement).

– Des vases cylindriques de mesure, béchers, entonnoirs à filtre, tiges, aiguilles, etc.

Three extractions are performed, each requiring measurement For each extraction, the paper should be cut into strips measuring approximately 50 mm by 10 mm A mass of about 20 g must be placed into a flat-bottomed 600 cm³ flask, to which additional components are added.

300 cm 3 d'eau distillée bouillante désionisée ou distillée répondant aux conditions de conductivité spécifiées à l'article 15.

Le mélange doit être conservé dans un bain de vapeur pendant 60 min ± 5 min; le goulot du flacon étant couvert d'un bécher simplement déposé sur le col.

The suspension should be suction-filtered through pre-extracted filter paper using a Buchner funnel A flat-ended rod is employed to compress the paper residue, maximizing the extraction of the liquid.

Le volume de l'extrait est mesuré et l'amas résiduel est pesé (W).

The extract is then transferred to a flask similar to the extraction flask and evaporated to dryness in a water bath; contamination is prevented by the presence of a large beaker.

(environ 250 cm 3 ) suspendu tête en bas sur le flacon.

Après séchage complet, on ajoute environ 20 cm 3 d'eau désionisée dans le flacon et le séchage est recommencé.

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17 Chloride content of aqueous extract

To ensure accurate test results, all apparatus must be thoroughly cleaned It is recommended to boil flasks, beakers, and funnels in de-ionized water after standard cleaning and rinsing Handling should be done with stainless steel tongs, and any forceps or scissors used for sample preparation should also be made of stainless steel and maintained in a clean condition.

NOTE See also note 2 of 15.2.

– A measuring device capable of measuring a d.c voltage in the range 0 mV to 300 mV with an accuracy of 2 mV (for example, an electronic voltmeter or potentiometer such as a pH-meter).

– A 600 cm 3 flat-bottom high-grade resistance glass or quartz flask.

– A glass micrometer syringe (method 1 only).

– A microburette graduated in 0,01 cm 3 divisions (method 2 only).

– Measuring cylinders, beakers, filter funnels, rods and needles, etc.

For each of the three extractions, a determination will be conducted using paper strips measuring approximately 50 mm by 10 mm About 20 g of the sample will be placed in a 600 cm³ flat-bottom flask, followed by the addition of approximately 300 cm³ of boiling de-ionized or distilled water that meets the conductivity standards outlined in clause 15.

The mixture shall be kept in a steam bath for 60 min ± 5 min, the mouth of the flask being covered by a loosely fitting beaker placed over the neck.

The suspension shall then be filtered using suction through a pre-extracted filter paper in a

Buchner funnel A flat-ended rod is used to compress the cake of paper residue in order to express as much extract as possible.

The volume of the extract shall be measured and the residual cake weighed (W).

The extract shall be returned to a flask similar to the extraction flask and evaporated to dryness in a hot-water bath; contamination is prevented by a large beaker (approximately

250 cm 3 ) suspended inverted over the flask.

When completely dry, approximately 20 cm 3 of de-ionized water shall be added to the flask and the drying repeated.

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The extracted residue is dissolved in approximately 5 cm³ of 10% HNO₃, then transferred to a 100 cm³ beaker The flask is rinsed twice with 5 cm³ of acetone, which is added to the beaker after each wash.

The chloride content of the extract is determined potentiometrically using a magnetic stirrer, a glass reference electrode, and a silver wire indicator, along with a measuring device such as a pH meter.

The titrant agent should be a 0.02 M solution of AgNO₃, added in increments of 0.01 cm³ using a micrometer syringe This should be done through a glass needle, dispensing dropwise into the titration cell.

Titrer un témoin composé comme suit: (340 – W) cm 3 d'eau après évaporation jusqu'à l'état sec, 5 cm 3 de HNO 3 à 10 % et 10 cm 3 d'acétone.

The chloride content of the extracted solution should be regarded as the mass of chloride ions, expressed in micrograms per gram of paper It can be calculated using the formula: chloride content (µg/g) = 35.46 (A B).

M est la molalité de la solution de AgNO3 en moles par kilogramme (mol/kg);

D est la masse de papier séché en grammes (g);

A est le volume de solution de AgNO 3 utilisée pour titrer l'extrait en centimètres cubes (cm 3) ;

B est le volume de solution de AgNO 3 utilisée pour titrer le témoin en centimètres cubes (cm 3) ;

W est la masse de résidu de papier humide en grammes (g);

V est le volume de l'extrait en centimètres cubes (cm 3)

Le résultat est la valeur médiane des trois déterminations.

Determination of the thickness of single sheets of paper (ISO 534)

The method is based on the use of a precision dial micrometer to measure the thickness of a single sheet when a static load is applied.

The static load to be applied shall correspond to a pressure of 100 kPa ± 10 kPa. b) Exceptions

The test will be conducted on three conditioned test pieces, with each piece undergoing one determination Each determination includes five measurements taken: one at each corner and one in the center of the test piece.

The results are given in microns.

Where thickness is determined across the width to establish the variation over the width, the details of this procedure will be found in IEC 60554-3.

Determination of mean thickness of paper

The method is based on the use of a precision dial micrometer to measure the thickness of a stack composed of a minimum of five sheets.

The static load to be applied shall correspond to a pressure of 100 kPa ± 10 kPa.

The test will be conducted on three conditioned samples, each made up of at least five sheets measuring 250 mm × 250 mm from a single specimen Each of the three samples will undergo one determination, which includes five measurements taken at each corner and one in the center of the test piece.

For narrow material where the width is less than the stipulated 250 mm, the five measurements on each stack shall be made at approximately equal intervals on a specimen measuring

The results are given in terms of the thickness of a single sheet in microns.

Where thickness is determined across the width to establish the variation over the width, the details of this procedure will be found in IEC 60554-3.

6 Substance (mass per square metre, basic weight or grammage)

Paper grammage shall be measured according to the method described in ISO 536 with the following exceptions:

– clauses 5 and 6 of ISO 536 are ignored;

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– l'essai doit être effectué sur trois éprouvettes conditionnées, une détermination étant faite sur chacune des trois éprouvettes;

– la masse doit être déterminée, à 0,5 % près, sur des éprouvettes conditionnées d'au moins

The surface area and mass of each specimen are measured, and the unit mass is calculated in grams per square meter, with all measurements taken on conditioned specimens.

Lorsque des mesures sont effectuées sur toute la largeur pour établir la variation transversale du grammage, les détails de ce mode opératoire seront indiqués dans la CEI 60554-3.

The thickness and grammage are determined for each of the three samples as outlined in Articles 5 and 6 For each sample, the apparent density is calculated, which is expressed in grams per cubic centimeter.

8 Résistance à la traction et allongement

La résistance à la traction et l'allongement doivent être mesurés conformément à l’une des méthodes décrites dans l'ISO 1924, avec les exceptions suivantes (la méthode à utiliser doit être indiquée dans la CEI 60554-3):

– des mesures sont effectuées sur neufs éprouvettes coupées dans le sens machine et sur neuf autres coupées dans le sens transversal;

– la valeur médiane des mesures, dans chaque sens, est prise comme résultat; les valeurs maximale et minimale dans chaque sens sont consignées;

– les résultats pourront éventuellement être exprimés sous forme de longueur de rupture, en mètres, arrondis à la tranche de 100 m la plus proche.

The measurement of the tensile force required to break 15 mm specimens, approximately 250 mm in length, cut in both directions of the paper, is conducted under standardized testing conditions.

The internal tear resistance must be measured according to the testing method outlined in ISO 1974 A simple tear resistance measuring device should be utilized, with the following exceptions.

– des mesures sont effectuées sur neuf éprouvettes coupées dans le sens machine et sur neuf autres dans le sens transversal.

Eprouvettes rectangulaires comportant une seule entaille, laissant une longueur de 43 mm à déchirer Mesure de l'énergie requise pour déchirer ces 43 mm.

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– the test shall be carried out on three conditioned test pieces, one determination being made on each of the three test pieces;

– the mass is to be determined to an accuracy of 0,5 % on conditioned test pieces of not less than 500 cm 2

The mass and area of each conditioned test piece are measured, allowing for the calculation of mass per unit area in grams per square meter.

Where grammage is determined across the width to establish the variation over the width, the details of this procedure will be found in IEC 60554-3.

The thickness and grammage of each of the three test pieces are assessed according to clauses 5 and 6 Additionally, the apparent density is calculated for each test piece, which is expressed in grams per cubic centimeter.

Tensile strength and elongation shall be measured according to one of the methods described in ISO 1924 with the following exceptions (the method to be used shall be indicated in

– measurements are made on nine test pieces cut from the machine direction and on nine others cut from the cross direction;

– the central value of the measurements, in each direction, is taken as the result and the highest and the lowest values in each direction are reported;

– alternatively, the results can be expressed as the breaking length in metres rounded to the nearest 100 m.

Measurement of the tensile force required to cause failure of test pieces 15 mm by approximately 250 mm, cut from both directions of the paper, when applied under standard test conditions.

Internal tearing resistance shall be measured according to the method described in ISO 1974.

The single-tear tester shall be used with the following exceptions:

– measurements are made on nine test pieces cut from the machine direction and nine others from the cross direction.

Rectangular test pieces having a single cut leaving 43 mm length to be torn Measurement of the energy required to tear this.

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10 Résistance au déchirement des bords

A tear strip clamp (see Figure 1) must be used, which is attached to the tensile testing machine as outlined in ISO 1924 The tear strip clamp consists of a thin steel plate (A) that serves as a vertical support, with its edge resting on the ends of a forked frame.

The thin metallic silk of the stirrup frame is secured in the lower jaw of the tensile testing device, aligning the vertical midline of the stirrup with an imaginary line connecting the central points of the upper and lower jaws The vertical plate can be removed from the stirrup frame, and two plates of different thicknesses are provided for testing papers of varying thicknesses One plate has a thickness of 1.25 mm ± 0.05 mm, while the other measures 2.50 mm ± 0.05 mm.

The edge of the plate features a shallow V-shaped notch, with the sides forming an angle of approximately 150° ± 1° The sides of the V-notch have a semi-circular cross-section and must be perfectly smooth and straight.

Nine test specimens should be cut in the machine direction and nine others in the cross direction of the paper; they must be between 15 mm and 25 mm wide and at least 250 mm long.

Les éprouvettes doivent être conditionnées conformément à l'article 4.

Fixer une plaque d'épaisseur convenable sur le bâti de l'étrier On montera la plaque de 1,25 mm ± 0,05 mm pour les papiers de 0,75 mm d'épaisseur maximale, et la plaque de

2,50 mm ± 0,05 mm pour les papiers plus épais.

Secure the thin silk of the stirrup in the lower jaw of the tensile testing device, ensuring that the vertical midline of the stirrup aligns with the imaginary line connecting the central points of the upper and lower jaws Additionally, position the sides of the V-notch symmetrically relative to the line that runs through these central points.

NOTE Si nécessaire, l'étrier pourra être fixé dans la mâchoire supérieure Dans ce cas, l'appareil d'essai de résistance à la traction sera rééquilibré pour compenser la masse de l'étrier.

Position the lower jaw of the device so that the lower edge of the upper jaw is approximately 90 mm above the upper edge of the plate with the V-notch.

Enfiler l'éprouvette dans l'étrier, sous la plaque, et réunir les deux extrémités en les fixant dans la mâchoire supérieure.

This operation will effectively reduce most of the slack in the specimen; however, care must be taken to avoid applying a tearing force Whenever possible, the initial increases in the load applied to the specimen should be done very gently to prevent abnormal stresses caused by inertia effects.

Augmenter la charge pour que le déchirement se produise entre 5 s et 15 s; consigner cette charge, exprimée en newtons.

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Test apparatus

An edge-tear stirrup, as illustrated in figure 1, must be utilized and connected to the tensile testing apparatus in accordance with ISO 1924 standards This stirrup features a thin steel plate (A) that acts as a vertical plate, supported at the edge by the ends of a stirrup-shaped frame.

The stirrup frame's thin metal tang is secured in the lower clamp of the tension testing machine, aligning its vertical center line with the midpoint connection of the upper and lower clamps A removable vertical plate is included with the stirrup frame, accompanied by two plates of varying thicknesses for different paper thickness ranges: one measuring 1.25 mm ± 0.05 mm and the other 2.50 mm ± 0.05 mm Each plate features a shallow V-notch with sides that form an angle of 150° ± 1°, and the V-notch sides are designed to be smooth and straight with a semicircular cross-section.

Test pieces

A total of eighteen test pieces will be prepared, with nine cut in the machine direction and nine in the cross direction of the paper Each piece will measure between 15 mm and 25 mm in width and will have a minimum length of 250 mm.

The test pieces shall be conditioned according to clause 4.

Procedure

Attach a plate of the proper thickness to the stirrup frame The plate with the thickness of

1,25 mm ± 0,05 mm is to be used for papers of up to 0,75 mm in thickness and the plate with the thickness of 2,50 mm ± 0,05 mm for thicker papers.

Secure the thin tang of the stirrup in the lower clamp of the tension-testing machine, ensuring that the vertical center line of the stirrup aligns with the line connecting the mid-points of the upper and lower clamps, while also positioning the sides of the V-notch symmetrically along this line.

NOTE The stirrup may be fastened in the upper clamp, if desired This procedure will require rebalancing the tension-testing machine to compensate for the mass of the stirrup.

Place the lower clamp of the machine so that the lower edge of the upper clamp is about

90 mm above the upper edge of the V-notched plate.

Thread the test piece through the stirrup, under the plate, and bring the two ends together and fasten them in the upper clamp.

During this operation, it is crucial to absorb most of the slack in the test piece without applying a tearing force To minimize abnormal strains caused by inertia effects, the initial increments of load should be applied to the test piece very slowly whenever possible.

Increase the load so that tearing starts in 5 s to 15 s and record this load in newtons.

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Record the median values, expressed in newtons, for both directions of the paper, noting the thickness of the plate used, the load application speed, as well as the width and thickness of the specimens.

La résistance à l'éclatement doit être déterminée conformément à la méthode décrite dans l'ISO 2758, avec les exceptions suivantes:

– les éprouvettes doivent être conditionnées conformément à l'article 4.

A test tube is rigidly attached to the perimeter of a circular elastic diaphragm while remaining free to bulge with it A hydraulic fluid is pumped at a constant rate to inflate the diaphragm until the test tube breaks The burst strength of the test tube is defined as the maximum value of the applied hydraulic pressure.

Un appareil d'essai de pliage (type Schopper).

Neuf bandes de 15 mm de large, découpées dans le sens machine, et neuf autres bandes découpées dans le sens transversal.

Clamp the test specimen between the two jaws Apply a tension of 5 N for specimens up to 0.03 mm thick, or 10 N for thicker specimens Determine the number of double folds the paper can withstand around a plate that is 0.5 mm thick with a curvature radius of 0.25 mm, at a speed of 100 to 200 double folds per minute.

Consigner la valeur médiane de chaque série, jusqu'à deux chiffres significatifs, ainsi que les valeurs maximale et minimale.

The moisture content of paper upon receipt must be measured according to the method outlined in ISO 287 (oven drying method) The result should be expressed as a percentage of moisture relative to the initial mass Three samples should be taken in accordance with ISO 287.

Peser l'éprouvette au moment de l'échantillonnage et, la peser de nouveau, après dessiccation jusqu'à masse constante, dans une étuve portée à une température comprise entre 102 °C et

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Results

The central values for both directions of the paper are reported in newtons, taking into account the plate thickness, loading rate, and the width and thickness of the test specimens.

The bursting strength shall be determined according to the method described in ISO 2758, with the following exceptions:

– the test pieces shall be conditioned in accordance with clause 4.

A test specimen is securely clamped around its edges while being in contact with a circular elastic diaphragm, allowing it to bulge as the diaphragm expands Hydraulic fluid is continuously pumped at a steady rate, causing the diaphragm to bulge until the test specimen fails The maximum hydraulic pressure applied at the moment of rupture determines the bursting strength of the test specimen.

Test apparatus

Test pieces

Nine strips 15 mm wide, cut in the machine direction, and nine other strips cut in the cross direction.

Procedure

To test the specimen, securely clamp it in both clamps and apply a tension of 5 N for specimens up to 0.03 mm thick, or 10 N for thicker specimens Measure the number of double folds the paper can endure by using a 0.5 mm thick plate with a 0.25 mm radius of curvature, at a speed of 100 to 200 double folds per minute.

Results

Report the central value of each series to two significant figures The highest and lowest values shall also be reported.

The moisture content of the received paper must be measured using the oven-drying method outlined in ISO 287, with results expressed as a percentage of the original mass Three test specimens should be collected in accordance with ISO 287 standards.

Weigh the test piece at the time of sampling and again after drying in an oven at 102 °C to

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La quantité de résidu de papier subsistant après l'incinération doit être déterminée confor- mément à la méthode décrite dans l'ISO 2144.

Il doit être procédé à trois déterminations Le résultat doit être exprimé en pourcentage de la masse séchée à l'étuve.

– Une cellule de mesure de la conductivité dont la constante K est connue.

A measuring device is capable of assessing conductance or inductance, with a minimum indication of 1 aS and an accuracy of 5%, across a frequency range of 50 Hz to 3000 Hz Additionally, resistance can be measured with the same level of precision.

– Des flacons coniques de 250 cm 3 , à large goulot, en verre résistant aux acides et aux alcalis, équipés de condenseurs à reflux.

The determination must be conducted on the material in its received state Three extractions should be performed, with each requiring a measurement A preliminary control test must be carried out using water that has been boiled for 60 minutes ± 5 minutes in the designated flask If the conductivity of this water does not exceed 200 µS/m, the flask may be used.

If the conductivity exceeds the specified value, it is necessary to boil a new quantity of water in the same flask Should the conductivity measured after the second test surpass 200 µS/m, a different flask must be used.

L'essai sur le papier doit être effectué comme suit.

Découper un échantillon, pesant environ 20 g, en morceaux d'environ 10 mm × 10 mm Peser

5 g de matière dans un flacon en verre de 250 cm 3 équipé d'un condenseur à reflux et ajouter

To ensure accurate results, 100 cm³ of water with a conductivity not exceeding 200 µS/m should be gently boiled for 60 minutes, with a tolerance of ± 5 minutes After boiling, allow the water to cool in the container to room temperature while taking precautions to prevent the absorption of carbon dioxide from the air.

The extract is then transferred to a measuring container for immediate conductivity determination The measuring container must be rinsed twice with the extract Conductivity measurements should be conducted at a temperature of 23°C ± 0.5 K.

NOTE 1 L'extraction selon la méthode 1 de l'article 17 peut être admise en variante, mais on utilisera alors 5 g dans 100 cm 3

During the collection, storage, and handling of samples and test tubes intended for conductivity, pH, and chloride content testing of aqueous extracts, it is crucial to prevent contamination from the atmosphere, particularly in a chemical laboratory, as well as from direct hand contact.

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The amount of residue of paper left after incineration shall be determined according to the method described in ISO 2144.

Three determinations shall be made The result shall be expressed as a percentage of the oven dry mass.

Test apparatus

– A conductivity cell with known cell constant K.

– A conductance or inductance measuring instrument, capable of measuring conductance to a minimum reading of 1 àS with an accuracy of 5 %, in the frequency range 50 Hz to 3 000 Hz.

Alternatively, the resistance may be measured with the same accuracy.

– Wide-mouth 250 cm 3 conical flasks with reflux condensers in acid- and alkali-resistant glass.

Procedure

The determination is based on the material as received, with one measurement taken from each of three extractions Initially, a blank test is performed using water that has been boiled for 60 minutes ± 5 minutes in the designated flask If the conductivity of this water is 200 µS/m or lower, the flask is deemed suitable for use However, if the conductivity exceeds this threshold, the flask must be boiled again with a new portion of water.

200 àS/m, then another flask shall be used.

The test on the paper shall then be carried out as follows.

Cut a test specimen weighing approximately 20 g into pieces of about 10 mm × 10 mm Weigh approximately 5 g into a 250 cm 3 glass flask with a reflux condenser and add approximately

To ensure accurate results, 100 cm³ of water with a conductivity not exceeding 200 µS/m should be gently boiled for 60 minutes, with a tolerance of ± 5 minutes, and then allowed to cool to room temperature in a flask It is essential to take precautions to prevent the absorption of carbon dioxide from the air during this process.

The extract is decanted into a measuring vessel for immediate conductivity measurement, which should be rinsed twice with the extract Conductivity measurements must be conducted at a temperature of 23 °C ± 0.5 K.

NOTE 1 Extraction in accordance with method 1 of clause 17 is an acceptable alternative, but 5 g in 100 cm 3 is to be used.

To prevent contamination during the collection, storage, and handling of specimens and test portions for conductivity, pH, and chloride content tests of aqueous extracts, it is crucial to avoid exposure to atmospheric pollutants, especially in a chemical laboratory, and to refrain from using bare hands during handling.

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Calculer la conductivité de la solution extraite comme suit: γ = K (G 1 – G 2 ) ó γ est la conductivitộ de l'extrait, exprimộe en microsiemens par mốtre (àS/m);

K est la constante de la cellule, exprimée en m –1 ;

G 1 est la conductance de l'extrait, exprimộe en microsiemens (àS);

G 2 est la conductance du tộmoin, exprimộe en microsiemens (àS).

– Un pH-mètre avec des électrodes en verre et en calomel ayant une sensibilité minimale de 0,05 unité pH.

– Des flacons coniques de 250 cm 3 , à large goulot, en verre résistant aux acides et aux alcalis.

Il doit être procédé à trois extractions dont chacune fera l'objet d'une mesure.

Préparer un extrait comme cela est décrit en 15.2.

The extract should only be transferred at the time of use to prevent unnecessary exposure to ambient air Calibrate the pH meter using a reference solution with a pH within ±2 units of the extract's pH After calibration, carefully rinse the electrodes in distilled water multiple times and once in a small amount of the extract.

Immerger les électrodes dans l'extrait non filtré et mesurer la valeur du pH de celui-ci à une température de 23 °C ± 2 K.

When using the extract to determine conductivity, it is essential to collect the sample from the aqueous extract prior to measuring the pH This is important because potassium chloride released by the calomel electrode could skew the results.

Consigner la valeur médiane comme étant le résultat; les valeurs maximale et minimale sont consignées.

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Results

Calculate the conductivity of the extract solution as follows: γ = K (G 1 – G 2 ) where γ is the conductivity of extract solution, expressed in microsiemens per metre (àS/m);

K is the cell constant, expressed in m –1 ;

G 1 is the conductance of the extract solution, expressed in microsiemens (àS);

G 2 is the conductance of the blank test, expressed in microsiemens (àS).

Test apparatus

– A pH-meter with glass and calomel electrodes having a sensitivity of at least 0,05 pH units.

– Wide-mouth 250 cm 3 conical flasks in acid- and alkali-resistant glass.

Procedure

One measurement shall be made on each of three extractions.

Prepare an extract as described in 15.2.

To ensure optimal results, decant the extract only for immediate use to minimize atmospheric exposure Calibrate the pH meter using a buffer solution with a pH value within ±2 units of the extract's pH After calibration, thoroughly rinse the electrodes in distilled water and then in a small amount of the extract.

Immerse the electrodes in the unfiltered extract and measure the pH value of the extract at

For accurate conductivity measurements, it is essential to collect the sample from the aqueous extract before determining the pH This is crucial as potassium chloride, which diffuses from the calomel electrode, can otherwise skew the results.

Results

Report the central value as the result; the highest and lowest values are reported.

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17 Teneur en chlorure de l'extrait aqueux

All equipment used during this experiment must be thoroughly clean It is recommended to boil all flasks, beakers, and funnels in deionized water after normal cleaning and rinsing The apparatus should be handled with stainless steel tongs Additionally, tweezers and scissors used for sample preparation should also be made of stainless steel and cleaned in the same manner.

NOTE Voir également note 2 de 15.2.

– Un appareil de mesure capable de mesurer une tension continue dans la gamme de 0 mV à

300 mV, avec une précision de 2 mV (par exemple un voltmètre électronique ou un potentiomètre tel qu'un pH-mètre).

– Un flacon en quartz ou en verre à haute résistance, à fond plat, d'une contenance de 600 cm 3

– Une seringue en verre à micromètre (pour la méthode 1 uniquement).

– Une microburette graduée en divisions de 0,01 cm 3 (pour la méthode 2 uniquement).

– Des vases cylindriques de mesure, béchers, entonnoirs à filtre, tiges, aiguilles, etc.

Three extractions are performed, each requiring measurement For each extraction, the paper should be cut into strips measuring approximately 50 mm by 10 mm About 20 grams of the sample must be placed in a flat-bottomed 600 cm³ flask, and approximately

300 cm 3 d'eau distillée bouillante désionisée ou distillée répondant aux conditions de conductivité spécifiées à l'article 15.

Le mélange doit être conservé dans un bain de vapeur pendant 60 min ± 5 min; le goulot du flacon étant couvert d'un bécher simplement déposé sur le col.

The suspension should be suction-filtered through pre-extracted filter paper using a Buchner funnel A flat-ended rod is employed to compress the paper residue, maximizing the extraction of the liquid.

Le volume de l'extrait est mesuré et l'amas résiduel est pesé (W).

The extract is then transferred to a flask similar to the extraction flask and evaporated to dryness in a water bath; contamination is prevented by the presence of a large beaker.

(environ 250 cm 3 ) suspendu tête en bas sur le flacon.

Après séchage complet, on ajoute environ 20 cm 3 d'eau désionisée dans le flacon et le séchage est recommencé.

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17 Chloride content of aqueous extract

Method 1

To ensure accurate test results, all apparatus must be thoroughly cleaned It is recommended to boil flasks, beakers, and funnels in de-ionized water after standard cleaning and rinsing Handling should be done using stainless steel tongs, and any forceps or scissors used for sample preparation should also be made of stainless steel and maintained in a clean condition.

NOTE See also note 2 of 15.2.

– A measuring device capable of measuring a d.c voltage in the range 0 mV to 300 mV with an accuracy of 2 mV (for example, an electronic voltmeter or potentiometer such as a pH-meter).

– A 600 cm 3 flat-bottom high-grade resistance glass or quartz flask.

– A glass micrometer syringe (method 1 only).

– A microburette graduated in 0,01 cm 3 divisions (method 2 only).

– Measuring cylinders, beakers, filter funnels, rods and needles, etc.

For each of the three extractions, a determination will be conducted The paper will be cut into strips measuring approximately 50 mm by 10 mm, and around 20 g of the material will be placed in a 600 cm³ flat-bottom flask Subsequently, approximately 300 cm³ of boiling de-ionized or distilled water, meeting the conductivity standards outlined in clause 15, will be added.

The mixture shall be kept in a steam bath for 60 min ± 5 min, the mouth of the flask being covered by a loosely fitting beaker placed over the neck.

The suspension shall then be filtered using suction through a pre-extracted filter paper in a

Buchner funnel A flat-ended rod is used to compress the cake of paper residue in order to express as much extract as possible.

The volume of the extract shall be measured and the residual cake weighed (W).

The extract shall be returned to a flask similar to the extraction flask and evaporated to dryness in a hot-water bath; contamination is prevented by a large beaker (approximately

250 cm 3 ) suspended inverted over the flask.

When completely dry, approximately 20 cm 3 of de-ionized water shall be added to the flask and the drying repeated.

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The extracted residue is dissolved in approximately 5 cm³ of 10% HNO₃, then transferred to a 100 cm³ beaker The flask is rinsed twice with 5 cm³ of acetone, which is added to the beaker after each wash.

The chloride content of the extract is determined potentiometrically using a magnetic stirrer, a glass reference electrode, and a silver wire indicator, along with a measuring device such as a pH meter.

The titrant agent should be a 0.02 M solution of AgNO₃, added in increments of 0.01 cm³ using a micrometer syringe with a glass needle, dripped into the titration cell.

Titrer un témoin composé comme suit: (340 – W) cm 3 d'eau après évaporation jusqu'à l'état sec, 5 cm 3 de HNO 3 à 10 % et 10 cm 3 d'acétone.

The chloride content of the extracted solution should be regarded as the mass of chloride ions, expressed in micrograms per gram of paper It can be calculated using the formula: chloride content (µg/g) = 35.46 (A B).

M est la molalité de la solution de AgNO3 en moles par kilogramme (mol/kg);

D est la masse de papier séché en grammes (g);

A est le volume de solution de AgNO 3 utilisée pour titrer l'extrait en centimètres cubes (cm 3) ;

B est le volume de solution de AgNO 3 utilisée pour titrer le témoin en centimètres cubes (cm 3) ;

W est la masse de résidu de papier humide en grammes (g);

V est le volume de l'extrait en centimètres cubes (cm 3)

Le résultat est la valeur médiane des trois déterminations.

17.2.1 Cette méthode s'écarte de la méthode 1 sur les points suivants:

– le traitement porte sur 4 g de papier dans 100 cm 3 au lieu de 20 g dans 300 cm 3 ;

– une ébullition intense est maintenue pendant 60 min ± 5 min;

The treatment of the extract is carried out as follows: First, filter or transfer the cooled extract solution and weigh 25 g ± 0.1 g in a tall, narrow 200 cm³ beaker Next, add 125 cm³ of acetone and 15 drops of 1% nitric acid Then, introduce a stirrer into the beaker and place it on a magnetic stirrer, adjusting the stirring speed to avoid breaking the liquid's surface Immerse the electrodes in the liquid and wait for the measurement device to stabilize before starting the titration Finally, using a microburette, add 0.0025 M AgNO₃ solution in small increments.

To conduct the titration, add 0.01 cm³ and record the potential change in millivolts (mV) Continue the titration until reaching the point of maximum potential change or a predetermined fixed point based on a potentiometric curve.

LICENSED TO MECON Limited - RANCHI/BANGALORE FOR INTERNAL USE AT THIS LOCATION ONLY, SUPPLIED BY BOOK SUPPLY BUREAU.

The extracted residue shall be dissolved in 5 cm 3 ± 1 % of 10 % HNO3, transferred to a 100 cm 3 beaker and the flask twice washed out into the beaker with 5 cm 3 ± 1 % of acetone.

The chloride content of the extract shall then be determined potentiometrically using a mag- netic stirrer, a glass reference electrode and a silver-wire indicator with a measuring device, for example, a pH-meter.

The titrant shall be a solution of AgNO 3 of 0,02 M added in quantities of 0,01 cm 3 from a micro- meter syringe through a glass needle dripping into the titration cell.

Titrate a reagent blank consisting of the following: (340 – W) cm3 of water evaporated to dryness, 5 cm 3 of 10 % HNO 3 , and 10 cm 3 acetone.

The chloride content of the extract solution is expressed as the mass of chloride ion in micrograms per gram of paper It is calculated using the formula: chloride content (10⁻⁶) = 35.46 (A B).

M is the molality of the AgNO3 solution in moles per kilogramme (mol/kg);

D is the mass of the dried paper in grams (g);

A is the volume of AgNO 3 solution used to titrate the extract in cubic centimetres (cm 3) ;

B is the volume of AgNO 3 solution used to titrate the blank in cubic centimetres (cm 3) ;

W is the mass of wet paper residue in grams (g);

V is the volume of extract in cubic centimetres (cm 3)

The result is the central value of the three determinations.

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