CRYSTAL GLASS ORDER (ORDER NO. 45 of 2000)

CRYSTAL GLASS

SUBSIDIARY LEGISLATION 427.04

CRYSTAL GLASS ORDER

(ORDER NO. 45 of 2000)

1st January, 2001

LEGAL NOTICE 184 of 2000, as amended by Legal Notice 302 of 2007.

1 The title of this Order is Crystal Glass Order, and may be

referred to as Order No. 45 of 2000.

Substituted by

L.N. 302 of 2007.

List of Crystal Glass categories

N

Description of

Labelling

Characteristics

category

o

Explanatory

Metal

Density

Refractive

Surface

Shape of

Remarks

notes

oxides(%)

index

hardness

symbol

a

b

c

d

e

f

g

h

i

≥ 3.00

1 FULL

LEAD

PbO

x

≥ 30%

CRYSTAL 30%

SUPERIEUR 30%

HOCHBLEI-

KRISTALL 30%

VOLLOOD-

KRISTALL 30%

Description

SUPERIORE 30% may be freely

used,

KRYSTAL 30%

whatever the

κρυoταλλα υψηλης c o u n t r y o f

περιεκτικoτητoς oε origin or the

country of

μoλυβδo 30%

destination.

SUPERIOR 30%

CHUMBO

SUPERIOR 30%

ТЕЖЪК ОЛОВЕН

КРИСТАЛ 30%

SUPERIOR 30%

≥ 2.90

2 LEAD CRYSTAL

PbO

x

≥ 24%

24%

PLOMB 24%

BLEIKRISTALL

24%

LOODKRISTALL

24%

CRISTALLO AL

PIOMBO 24%

The

KRYSTAL 24%

percentage

μ o λυβδ o υχα

figure refers

κρυoταλλα 25%

to the lead

ΜOΔYBΔOYXA oxide content

24%

PLOMO 24%

CHUMBO 24%

Round

label

ОЛ О В Е Н

КРИСТАЛ 24%

Colour

gold

Ø ≥ 1 cm

PLUMB 24%

N

Description of

Labelling

Characteristics

category

o

Explanatory

Metal

Density

Refractive

Surface

Shape of

Remarks

notes

oxides(%)

index

hardness

symbol

a

b

c

d

e

f

g

h

i

≥ 2.45

3 C RY S TA L

ZnO

nD≥ 1.520

Square

GLASS,

BaO

label

CRYSTALLIN

PbO

K 2 O

CRISTALLIN

Colour

single or

VETRO

silver

together

SONORO

≥ 10%

SUPERIORE

Side

KRISTALLGLAS

≥ 1 cm

GLAS (2)

SONOORGLAS

(3)

KRYSTALLIN

υαλoκρυoταλλα

VIDRIO

SONORO

SUPERIOR

VIDRO SONORO

SUPERIOR

КРИСТАЛИН

STICLÃ

CRISTALINÃ

≥ 2.40

4 C RY S TA L

Only

the

BaO

Vickers -

Label in

GLASS,

description in

PbO

550 ±20

the shape

CRYSTALLIN

the English

K 2 O

of an

VERRE SONORE l a n g u a g e

single or

equila-

may be used

together

teral

VETRO

≥ 10%

triangle

SONORO

KRISTALLGLAS

Colour

SONOORGLAS

silver

KRYSTALLIN

Side

υαλoκρυoταλλα

≥ 1 cm

VIDRIO

SONORO

VIDRO SONORO

СТЪКЛО

-

STICLÃ SONORÃ

x: nD ≥ 1.545 as criterion for an additional non-destructive determination of the products (at the time

of import).

(2) In Belgium

(3) In the Netherlands.

1 This Mandatory Order shall apply to the products falling

within heading No. 70.13 of the Common Customs Tariff.

2.2 This Mandatory Order shall not apply to products intended

exclusively for export.

Methods for determining the chemical and physical properties of categories of

crystal glass

1. CHEMICAL ANALYSES

1.1

BaO and PbO

1.1.1 Determination of the combination BaO + PbO

Weigh, to within 0.0001 grammes, approximately 0-5 grammes of powdered

glass and place in a platinum dish. Moisten with water and add 10 millilitres of a

15% solution of sulphuric acid and 10 millilitres hydrofluoric acid. Heat in a sand

bath until white fumes are given off. Allow to cool and treat again with 10 millilitres

hydrofluoric acid. Heat until reappearance of white fumes. Allow to cool and rinse

the sides of the dish with water. Heat until reappearance of white fumes. Allow to

cool, carefully add 10 millilitres of water, then transfer to a 400 millilitres beaker.

Rinse the dish several times with a 10% sulphuric acid solution and dilute to 100

millilitres with same solution. Boil for 2-3 minutes. Leave to stand overnight.

Pass through a filtering crucible of 4 porosity, wash first of all with a 10%

solution of sulphuric acid, then two or three times with ethyl alcohol. Dry for one

hour in an oven at 150ºC. Weigh BaSO 4 + PbSO 4 .

1.1.2 Determination of BaO

Weigh, to within 0.0001 grams, about 0-5 grams of powdered glass and

place in a platinum dish. Moisten with water and add 10 millilitres of hydrofluoric

acid and 5 millilitres perchloric acid. Heat in sand bath until white fumes are given

off.

Allow to cool and add a further 10 millilitres hydrofluoric acid. Heat until

reappearance of white fumes. Allow to cool and rinse the sides of the dish with

distilled water. Heat again and evaporate until almost dry. Start again with 50

millilitres of a 10% solution of hydrochloric acid and heat gently to aid dissolution.

Transfer to a 400 millilitres beaker and dilute to 200 millilitres with water. Bring to

boil and pass a current of hydrogen sulphide through the hot solution. When the

precipitate of lead sulphide drops to the bottom of the beaker, turn off the hydrogen

sulphide. Pass through a fine filter paper and wash with cold water saturated with

hydrogen sulphide.

Boil the filtrates and then, if necessary, reduce them by evaporation to 300

millilitres. Add to boiling mixture 10 millilitres of a 10% solution of sulphuric acid.

Remove from heat and leave to stand for at least four hours.

Pass through a fine filter paper, wash with cold water. Calcine the precipitate

to 1050ºC, and weigh the BaSO 4 .

1.2

Determination of ZnO

Evaporate the filtrates from the separation of BaSO 4 so as to reduce their

volume to 200 millilitres. Neutralise with ammonia in the presence of methyl red and

add 20 millilitres of N/10 sulphuric acid. Adjust the pH to 2 (pH meter) by adding N/

10 sulphuric acid or N/10 caustic soda whichever the case, and precipitate the zinc

sulphide in the cold by passing a current of hydrogen sulphide. Let the precipitate

settle for four hours, then collect on a fine filter paper. Wash with cold water

saturated with hydrogen sulphide. Dissolve the precipitate on the filter by pouring

through it 25 millilitres of a hot 10% solution of hydrochloric acid. Wash the filter

with boiling water until a volume of about 150 millilitres is obtained. Neutralise with

ammonia in the presence of litmus paper, then add 1-2 grams solid urotropine to

buffer the solution to about pH 5. Add a few drops of a 0-5% freshly prepared

aqueous solution of xylenol orange and titrate with an N/10 solution of Complexon

III until the pink changes to citron yellow.

1.3

Determination of K 2 O

by precipitation and weighing of potassium tetraphenylborate

Procedure: 2 grammes of glass are attacked, after crushing and sieving, by

2 millilitres concentrated HNO 3

15 millilitres HC10 4

25 millilitres HF

in a platinum dish on a water-bath then in a sand bath. After dense fumes of

perchloric acid have been given off (continue until dry), dissolve with 20 millilitres

of hot water and 2-3 milllitres concentrated HCl.

Transfer to a 200 millilitres graduated flask and adjust to volume with

distilled water.

Reagents: 6% solution of sodium tetraphenylborate: dissolve 1.5 grams of

the reagent in 250 millilitres distilled water. Remove the light cloudiness which

remains by adding 1 gram of hydrated alumina. Shake for five minutes and filter,

taking care to re-filter the first 20 millilitres obtained.

Washing solution for the precipitate: prepare a little of the potassium salt by

precipitation in a solution of about 0.1 grams KCl to 50 millilitres N/10 HCl into

which the solution of tetraphenylborate is poured while stirring, until precipitation

ceases. Filter through a sinter. Wash with distilled water. Dry in a desiccator at room

temperature. Then pour 20-30 milligrams of that salt into 250 millilitres of distilled

water. Stir from time to time. After thirty minutes, add 0.5-1 gram of hydrated

alumina. Stir for a few minutes. Filter.

Method of operation: Take an aliquot of the acid digest corresponding to about 10

milligrams of K 2 O. Dilute to about 100 millilitres Slowly add the reagent solution,

about 10 millilitres per assumed 5 milligrams of K 2 O, while gently stirring. Allow to

stand for a maximum of fifteen minutes then filter through a tared sintered crucible

of porosity 3 or 4. Wash with washing solution. Dry for thirty minutes at 120ºC.

Conversion factor 0.13143 for K 2 O.

1.4

Tolerances

± 0.1 in absolute value for each determination. If the analysis gives a lower

value, within the tolerances, than the limits fixed (30, 24 or 10%), the average of at

least three analyses must be taken. If that average is greater than or equal to 29.95,

1 The composition, characteristics of manufacture and

labelling of the products referred to in paragraph 2.1, and all forms

of publicity for such products shall conform to the definitions and

rules laid down in this Order and in the Schedules thereto.

3.2 The descriptions in column (b) of the First Schedule may

not be used commercially for products which do not have the

corresponding characteristics specified in columns (d) to (g) of the

First Schedule.

3.3 If a product covered by this Order bears one of the

descriptions listed in column (b) of the First Schedule, it may also

bear the corresponding identifying symbol shown and described in

columns (h) and (i) of the First Schedule.

3.4 Where a trade mark, the name of an undertaking or any

other inscription contains, as a main part, as an adjective or as a

root, a description appearing in columns (b) and (c) of the First

Schedule or a description liable to be confused therewith, the trade

mark, name or inscription shall immediately be preceded by the

following, in very prominent lettering

(a) the description of the product, where that product has

characteristics specified in columns (d) to (g) of the

First Schedule;

(b) a statement of the exact nature of the product, where

that product does not have characteristics specified in

columns (d) to (g) of the First Schedule.

3.5 The description and identifying symbols given in the First

Schedule may appear on one and the same label.

1 The methods laid down in the Second Schedule, and only

those methods, shall be used to verify that products bearing

descriptions and identifying symbols have the characteristics

corresponding thereto as specified in columns (d) to (g) of the First

Schedule.

95 or 9.95 respectively, the glass must be accepted in the category corresponding

to 30, 24 and 10% respectively.

2. PHYSICAL DETERMINATIONS

2.1

Density

Method by hydrostatic balance to within ± 0.01. A sample of at least 20

grams is weighed in air and weighed immersed in distilled water at 20ºC.

2.2

Refractive index

The index is measured on the refractometer to within ± 0.001.

2.3

Microhardness

Vickers hardness is to be measured according to the standard ASTM E 92-65

(Revision 1965) but using a load of 50 grams and taking an average of 15

determinations.