S.I. No. 81/1952 - Standard Specification (Writing Ink) Order, 1952.


S.I. No. 81 of 1952.

STANDARD SPECIFICATION (WRITING INK) ORDER, 1952.

I, SEAN F. LEMASS, Minister for Industry and Commerce, in exercise of the power conferred on me by subsection (3) of section 20 of the Industrial Research and Standards Act, 1946 (No. 25 of 1946), hereby order as follows:—

1. This Order may be cited as the Standard Specification (Writing Ink) Order, 1952.

2.—(1) The specification set forth in Part II of the Schedule to this Order is hereby declared to be the standard specification for the commodity described in Part I of the said Schedule.

(2) The said standard specification may be cited as Irish Standard 38: 1952.

SCHEDULE.

PART I.

WRITING INK.

PART II.

SPECIFICATION.

SCOPE.

1. This specification covers the requirements of blue-black writing inks which are suitable for use in fountain pens and dip pens.

REFERENCE INK.

2. The reference ink used for the purpose of testing inks for compliance with this specification shall be prepared as described in Appendix A. The reference ink shall be prepared not more than three months before use.

SEDIMENT.

3. The ink shall be clear and free from sediment when examined visually as described in Appendix B.

STABILITY.

4. The ink, when treated as described in Appendix C and compared with the reference ink similarly treated, shall be as free from mould and deposit as the reference ink.

CORROSIVE ACTION.

5. The ink, when tested as described in Appendix D, shall not cause a greater loss in the weight of a steel nib than the reference ink.

WRITING PROPERTIES.

6. When written with, the ink shall not smudge or be sticky after drying, and shall not penetrate unreasonably through good quality writing paper. It shall produce clear characters having sufficient intensity of colour when blotted.

IRON CONTENT.

7. The iron content of the ink, expressed as metallic iron, shall be not less than 1ù5 g. per litre, and not more than 3ù5 g. per litre.

COMPOSITION.

8. The ink, when tested as described in Appendix E, shall conform to the following requirements:

the total soluble solids shall be not more than 4.5 g. per 100 ml. of ink,

free sulphuric acid expressed as barium sulphate shall be not more than 0.5 g. per 100 ml. of ink,

free hydrochloric acid shall be not more than 0.25 g. per 100 ml. of ink.

FORM AND COLOUR OF INK STREAKS.

9. Streaks of the ink, when freshly made as described in Appendix F and allowed to dry, shall show, when compared with streaks of the reference ink similarly made,

(a) the same general form,

(b) no greater evidence of feathering or striking through the paper,

(c) as uniform a colour when viewed from the front and the back, and

(d) as intense a colour when kept in diffused daylight for one week.

PERMANENCE OF INK STREAKS TO LIGHT.

10. The ink streaks, when tested for permanence to light as described in Appendix G, shall show no greater evidence of fading than those of the reference ink.

RESISTANCE OF INK STREAKS TO SOAKING.

11. The ink streaks, when tested as described in Appendix H, shall show no greater loss of colour than those of the reference ink.

RESISTANCE OF INK STREAKS TO BLEACHING.

12. The ink streaks, when tested as described in Appendix J and examined after periods of 15 minutes, 1 hour and 24 hours, shall show no greater loss of colour than those of the reference ink.

CONTAINERS.

13. The ink shall be packed in suitable containers which shall not change the composition of the ink nor be corroded by the components of the ink. The containers shall be of any of the following sizes: 1, 2, 4, 10, 20, 40 fluid ounces.

KEEPING PROPERTIES.

14. The ink shall have such keeping qualities that it will not deteriorate when stored in its container for one year.

MARKING.

15. Each container shall be clearly marked with the name of the ink, the name or mark of the manufacturer and the net contents in fluid ounces.

SAMPLING.

16. For the purpose of testing conformity with this specification a sample shall be taken at random from at least one in every ten containers or from every container if the number is less than ten. Before taking a sample the ink in the container shall be thoroughly mixed. The size of the sample shall be one fluid ounce for every five gallons of ink. The combined samples shall be mixed together and from the total a sample of at least one pint shall be taken and shall be packed in a glass container. The container so filled shall be sealed and shall be marked with the date of sampling and with sufficient information to identify the sample.

Appendix A.

PREPARATION OF STANDARD REFERENCE INK.

The ingredients used in preparing the reference ink shall be as follows :

Tannic acid

11·7 g.

Gallic acid crystals

3·8 g.

Ferrous sulphate (FeSO4.7H2O)

15·0 g.

Hydrochloric acid (10% by weight)

12·5 g.

Carbolic acid (Phenol)

1·0 g.

Soluble Blue (British Colour Index No. 707 of the Society of Dyers and Colourists)

3·5 g.

Distilled water to make a volume of 1 litre at 20°C.

All the ingredients except the dye shall be of the strength and quality prescribed by the British Pharmacopœia. The dye shall be of such quality that the ink when made as described in this Appendix shall show no sediment when kept in partly filled bottles for six months.

As ferrous sulphate crystals lose water of crystallization, a correction factor shall be employed in weighing out the ferrous sulphate. The correction factor shall be determined by estimating the iron in the ferrous sulphate by any suitable analytical method.

The appropriate quantities of gallic and tannic acids shall be weighed out and dissolved in 300 ml. distilled water at 60°C. The solution shall be filtered while hot and the beaker and paper shall be washed three times with hot distilled water. The correct amount of ferrous sulphate determined as described above shall be weighed out, and added to the solution. The flask shall be shaken to effect solution.

The requisite amount of hydrochloric acid shall then be added. The appropriate quantity of phenol shall be dissolved in the minimum quantity of water and added to the solution. The mixture shall then be cooled to room temperature and the blue dye shall be weighed out, dissolved in distilled water, filtered, and added to the solution. The solution shall then be mixed well and sufficient water shall be added to bring the total volume to 1 litre. The solution shall then be filtered through a Buchner filter and stored in clean stoppered bottles away from light. In order to exclude air the bottles should be filled as completely as possible.

Appendix B.

DETERMINATION OF FREEDOM FROM SEDIMENT.

The sample of ink taken in accordance with Clause 16 shall be allowed to stand for 24 hours to permit any solid matter to settle. The bottle shall then be held up against the light and slowly tilted away from the observer, who can thus detect sediment, if any, on the bottom of the bottle.

Appendix C.

DETERMINATION OF STABILITY.

Twenty-five ml. of the ink and 25 ml. of the reference ink shall be allowed to stand undisturbed each in a 50 ml. beaker covered by a watch glass. The inks shall be exposed to diffused daylight at room temperature for two weeks and shall then be compared for freedom from mould and deposit.

Appendix D.

DETERMINATION OF CORROSIVE ACTION.

Two new nibs shall be selected from the same box of ordinary non-stainless steel nibs. The nibs shall be cleaned with alcohol and with ether and dried in an oven at 105° C. Each of the nibs shall be weighed to the nearest milligram. Twenty-five ml. of the ink under test and 25 ml. of the reference ink shall be placed in similar small loosely-stoppered flasks. One nib shall be placed in each vessel of ink. During these operations the nibs shall be handled with a forceps.

After 48 hours the nibs shall be removed, scrubbed with water and cleansed thoroughly. They shall be rinsed with alcohol, dried in an oven at 105° C., cooled and weighed. The losses in weight of the two nibs shall be compared.

Appendix E.

DETERMINATION OF COMPOSITION.

Total soluble solids : Ten ml. of the ink shall be placed in a tared porcelain basin of 50 ml. capacity, evaporated and dried to constant weight on a steam bath. From the result the weight of the residue in grams per 100 ml. of ink shall be calculated.

Free sulphuric acid : Ten ml. of the ink shall be placed in a platinum dish of 50 ml. capacity and 10 ml. of a 10 per cent. solution of sodium carbonate shall be added and the contents of the dish evaporated to dryness on a steam bath. The residue shall be heated for one hour in an air-oven at 120°C. and shall then be ignited at 700° C. to 750° C. for half-an-hour. To the cooled platinum dish 30 ml. of distilled water and 5 ml. of a saturated solution of bromine water shall be added. The dish shall be heated for an hour on a steam bath and the contents filtered. The dish and the residue on the filter paper shall be washed with a 1 per cent. sodium carbonate solution. The beaker containing the filtrate shall be covered with a clock-glass and sufficient 4N hydrochloric acid shall be added to render the solution slightly acid. The bromine shall then be driven off by heating on a steam bath for one hour.

Ten ml. of 10 per cent. barium chloride solution shall be added to the boiling solution and it shall be allowed to stand until the precipitate becomes granular. The solution shall be filtered through an ashless filter paper. The residue shall be washed free from soluble salts, dried and ignited in a weighed crucible. The crucible shall be cooled and weighed. The heating and cooling shall be repeated until the weight is constant.

A blank test shall be carried out on the reagents and the necessary correction made to the weight of barium sulphate. The weight so corrected shall be multiplied by 10 to obtain the weight of barium sulphate precipitated from 100 ml. of the ink. The weight of free sulphuric acid, expressed as barium sulphate, shall be taken as the weight of barium sulphate precipitated from 100 ml. of the ink minus 4·18 times the content of metallic iron per 100 ml. of ink.

Free hydrochloric acid : Ten ml. of the ink shall be placed in a platinum dish of 50 ml. capacity and 10 ml. of a 10 per cent. solution of sodium carbonate shall be added and the contents of the dish evaporated to dryness on a steam bath. The residue shall be heated for one hour in an air-oven at 120° C. and shall then be ignited at 700° C. to 750° C. for half-an-hour and allowed to cool. Thirty ml. of distilled water shall then be added to the residue and the dish heated for one hour on a steam bath.

The solution shall be filtered and the dish and precipitate shall be washed with a 1 per cent. sodium carbonate solution. The beaker containing the filtrate shall be covered with a clock-glass and sufficient 4N nitric acid shall be added to render the solution acid and the solution boiled to expel carbon dioxide. The solution shall be made alkaline with ammonia to check the removal of iron and filtered if necessary. The solution shall then be acidified with nitric acid, and a solution of approximately 0·1N silver nitrate shall be added. The solution shall be heated to coagulate the precipitated silver chloride which shall then be collected in a clean dry tared Gooch crucible The precipitate shall be washed with water containing nitric acid and shall be dried at 150° C. to constant weight.

From the result the weight of silver chloride precipitated from 100 ml. of the ink shall be calculated. The content of free hydrochloric acid shall then be determined by multiplying the value obtained by 0·254.

Appendix F.

PREPARATION OF INK STREAKS.

A sheet of white bond paper shall be clamped to a sheet of glass so that it projects 3/8 in. below the glass. The glass shall be inclined at an angle of 45 degrees to the vertical.

The paper shall be placed so that the machine direction of the paper lies along the slope of the glass. To determine the machine direction of the paper a one inch square of the paper shall be laid on a surface of water. Two opposite edges of the paper will curl up to form a shallow trough and the axis of this trough shall be taken as parallel to the machine direction of the paper.

A pipette containing 1 ml. of the ink shall be held in a vertical position with the nozzle just touching the paper at the top of the sheet and the ink allowed to flow slowly down the paper so that a straight streak of uniform width and intensity is produced. In a similar manner a streak shall be made with the reference ink so that the two streaks are 1 in. apart. This procedure shall then be repeated making 3 streaks with the ink to be tested and 3 with the reference ink.

The streaks shall be kept in diffused daylight for one week to allow the colour of the inks to develop.

The bottom ½ in. of the sheet shall then be cut off and discarded and 5 strips each 1 in. in width shall be cut off at right angles to the streaks starting at the bottom of the sheet. These strips shall be numbered 1, 2, 3, 4 and 5, respectively. All of the strips and the remainder of the sheet shall be stored away from light and laboratory fumes.

The strips Nos. 1 and 3 shall be used for the determination of resistance to soaking. Strip No. 4 shall be used for the determination of resistance to bleaching. Strip No. 5 shall be used for the determination of permanence to light.

Appendix G.

DETERMINATION OF PERMANENCE TO LIGHT.

The test strip No. 5, prepared as described in Appendix F, shall be exposed in a window facing south for 14 days. The streaks made with the ink under test shall then be compared visually with the streaks made with the reference ink.

Appendix H.

DETERMINATION OF RESISTANCE TO SOAKING.

The test strips Nos. 1 and 3, prepared as described in Appendix F, shall be used for this test. One of these strips shall be soaked in distilled water for 24 hours and the other in 50 per cent. alcohol solution for the same period. The strips shall then be dried in air and the streaks made with the ink under test shall be compared with those made with the reference ink for each strip.

Appendix J.

DETERMINATION OF RESISTANCE TO BLEACHING.

A solution of bleaching powder of N/200 with respect to the available chlorine, shall be used for this test.

Test strip No. 4, prepared as described in Appendix F, shall be immersed in 100 ml. of the bleaching powder solution placed in a 250 ml. beaker.

The colour of the ink under test shall be compared with the colour of the reference ink after periods of immersion of 15 minutes, 1 hour and 24 hours.

GIVEN under my Official Seal this 31st day of March, 1952.

SEAN F. LEMASS,

Minister for Industry and Commerce.