Manual on

Chemical Analysis Methods

in Galvanizing
Content
1. Degreaser ( starts page 2)

2. Acid Pickle ( starts page 4)

3. Flux ( starts page 9)

4. Chromate Passivation ( starts page 21)

5. Zinc Bath analysis ( not included in this document)

6 Appendix 1 ( starts page 25)

7 Appendix 2 ( starts page 30)

8 Appendix 3 (starts page 31)

BRIEF SUMMARY OF MANUAL CONTENTS

The reaction between molten zinc and steel to form a continuous adherent coating can only occur if the steel
surface is free from foreign materials such as oil, grease, paint, rust, millscale and dirt of various kinds. A correctly
prepared surface is obtained by pretreating the steel surface with solutions which remove the foreign materials
and replaces them with a thin layer of flux. Cool down of the galvanized article is generally conducted in a water
tank to which additions of sodium dichromate passivator are made for the purpose of reducing the risk of white
rusting.

These process solutions will only work effectively and efficiently if they are of the correct composition and it is
important that proper control procedures be used to maintain the compositions of the solutions during their
working life.

Galvanizing Process Solutions

This manual covers the following process solutions (liquors);

• Degreaser
• Acid pickle
• Preflux
• Quench

And provides information on:

• The function of each liquor.

• The operating conditions and procedures to adjust each liquor.

• The procedures used to analyse each liquor.

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1. DEGREASER
1.1 Introductory Comments

This solution is used to remove oil and greases from the steel surface. The following information refers specifically
to caustic soda based degreasing solutions which are the most commonly used in practice.

The speed at which steel articles are cleaned is dependent on temperature and sodium hydroxide content. The
solution is usually heated between 50-70ºC and the sodium hydroxide content is usually maintained between 50-
100g/L. Some commercially available degreasers may contain additional cleaning agents to improve the cleaning
efficiency and extend the life of the bath.

For optimum performance, two properties need to be monitored and adjusted as necessary. These are;

 Free alkali
This is the alkali available for cleaning. This is the sodium hydroxide content.

 Total alkali
This is the sum of the free alkali and the combined alkali. The combined alkali is the alkali
which is combined with the soil and is not available for cleaning.

 The ratio of free alkali to total alkali is used to give an indication of the cleaning capacity. It indicates how
much free alkali is remaining to remove the soil as a proportion of the total alkali. For example, a high
ratio of 0.9 shows that there is a large amount of alkali available for cleaning whereas a ratio of 0.5 shows
that there is a low level of free alkali so the cleaning capacity is low.

As the bath ages, the proportion of by-products increases and thus the ratio of free alkali to total alkali decreases.
The ratio should always be maintained above 0.5 by additions of fresh degreaser. When the amount of by-
products build up to a level where the ratio cannot be maintained above 0.5 the solution may need to be partially
or totally dumped.

Although zinc may be present in the degreaser from carry-over from work jigs, it is not usually present at high
levels so is not considered a problem.

1.2 Summary of Recommended Operating Conditions for the Degreaser

Temperature Working Range: 70 - 90ºC

 Sodium Hydroxide Content (NaOH) Working Range: 50 - 100g/L

Ratio (“Free” to “Total Alkali”) is minimum 0.5

Any proprietary additions to the degreaser must be maintained according to the suppliers’ instructions.

1.3 Analysis Procedures for the Degreaser

On a routine basis, eg, once a month, analysis needs to be made of free alkali (sodium hydroxide) and total alkali,
from which the ratio can be determined. Then adjustment to the solution can be made accordingly to ensure
operating conditions as above are maintained. The test procedures are outlined on the following pages which
include;

1. Sodium hydroxide content, ie, the “free alkali” content (Section 1.3.1).
2. Ratio determination (Section 1.3.1).

1.3.1 Sodium Hydroxide Content and Ratio Determination

Equipment Required

-100ml measuring cylinder

-50mL burette
-250mL conical flask
-adjustable pipettor (adjust to 1mL)
-100mL plastic bottle with a screw top lid
Reagents Required (see preparation of these in Appendix 2)
- 1L 0.1N hydrochloric acid
- 100mL phenolphthalein indicator
- 100mL bromocresol green indicator

Method

1 Take a sample of about 100mL from the degreasing bath in a plastic bottle and allow it to stand to cool to
room temperature and to settle any sediment.
2 Using the clean pipettor, take 1mL of solution from the sample and transfer it into the clean conical flask, add
about 100mL of water, and add a few drops of phenolphthalein indicator. The solution will turn pink.
3 Fill the clean burette to the zero mark with 0.1N hydrochloric acid and titrate slowly with this solution, while
swirling the conical flask, until the pink colour vanishes.
4 Record the burette reading. This is the first endpoint (Titration, A).
5 To the above solution add a few drops of bromocresol green indicator. The solution will turn blue.
6 Continue titrating slowly with the standard 0.1N hydrochloric acid until the solution turns permanent yellow.
7 Record the burette reading. This is the second endpoint (Titration, B).

Calculation
Sodium Hydroxide Content (NaOH) If the bath contains caustic soda only, then its concentration is calculated as
follows; Where A is the first titration endpoint and B is the second titration endpoint the sodium hydroxide
content is; NaOH g/L = [A – (B – A)] x 4.0 If the bath is a proprietary solution, this can only be used as a guide. For
formulated baths the factor will not be 4.0 but one specific to the product, usually between 5.5 - 7.0.
Ratio Determination Gives an indication of the cleaning capacity of the bath and is calculated as follows;

Ratio = Titration A Titration B

Example

If the titration to the first endpoint is 22mL and the titration to the second endpoint is 24mL, then

NaOH g/L = [22 – (24-22)] x 4.0 = [22 - 2] x 4.0 = 20 x 4.0 = 80.0g/L Ratio = 22 /24 = 0.92

Quality Check : Using the above method, check the accuracy of the results with the standard sodium hydroxide
solution. Preparation of this standard solution is outlined in Appendix 3 .

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2 ACID PICKLE
2.1 Introductory Comments

The acid pickle is used to remove rust, millscale and other iron oxides from the steel surface. The following
information refers specifically to hydrochloric acid pickling as this is the most commonly used acid in galvanizing
plants. Hydrochloric acid is normally used at ambient temperature. The efficiency of the pickle depends on free
acid concentration, iron content and acid circulation (agitation). Recommended normal practice is to start with
approximately 15% (150g/L) acid concentration. Commercially supplied hydrochloric acid is typically 28-30%
concentration, which means diluting this 1:1 with water.

During use, two changes occur: the free acid content decreases and the iron content increases

There exits for any free acid content an optimum iron content for pickling efficiency. The optimum pickle
tank management practice is to use the Kleingarn Method as discussed below. This method is based on
the fact that for a given level of acid concentration, there exists:

1. An upper iron (Fe) content above which the acid can no longer dissolve more Fe. This is the
saturation Fe content. Pickling therefore completely stops above this limit no matter what the
acid concentration is. For example adding fresh concentrated acid will not improve the situation
2. For any acid concentration there is an Fe content at which the pickling rate is optimal. Above or
below this Fe content the pickling speed reduces
3. The above relationships between acid content, iron content and pickling rate are defined by the
Kleingarn Diagram ( see below)

The optimum Kleingarn procedure for acid pickle tank management is as follows

 For a new pickle tank, and starting with commercial grade HCl which is usually 32% concentration,
dilute this 1:1 with water to achieve a 16% HCl concentration in the tank

 The acid content should be maintained at approx 16% only until the Fe content reaches the
optimum pickling line in the diagram. Acid additions are then temporarily stopped, the acid % will
decrease and Fe content will continue to increase as pickling continues.
 Adjustments to bring the Fe content and acid % back to the optimum line are then made ( with fresh
acid or water additions ).

 Such adjustments are continued until the acid % reduces to 6% and the Fe content reaches 145g/L.
Pickling then becomes much slower and the acid can only then be used for zinc stripping
 KLEINGARN DIAGRAM (THE YELLOW OUTLINED AREA IS THE OPTIMAL WORKING RANGE FOR
MAXIMUM PICKLING EFFICIENCY)

Optimum pickling time

Pickling not possible above the Fe saturation

line

Fe saturation line (the

acid cannot dissolve any
Iron more Fe)
content
g/L

Arrows point in
the
direction of
increasing
pickling speed

Pickling is
possible below the
shaded area but with a
longer pickling time

Hydrochloric acid concentration g/L

THE YELLOW OUTLINED AREA IS THE OPTIMAL WORKING RANGE FOR MAXIMUM PICKLING
EFFICIENCY

Agitation of steelwork in the pickling tank, or forced circulation of acid (pumping), will considerably improve the
pickling rate due to removal of iron build-up in the pickle adjacent to the steel surface which would otherwise
have a partial inhibiting effect on the pickling reaction.

Zinc contamination in operating pickling baths, for example from work jigs/rework, should be avoided if possible
as it reduces significantly the rate of pickling of steel surfaces. For this reason, if possible, attempt to limit any zinc
contamination to only one operating tank and one which has been in service for an extended period of time (ie.
iron content is high).

2.2 Summary of Recommended Operating Conditions for the Acid Pickle

 Temperature Working Range ambient temperature (approx. 20-30ºC)

 Hydrochloric Acid Content (HCl) New Solution: 150 - 160g/L (15 -16%) Optimum Operation as per Kleingarn

Diagram ( range is 16% - 6% depending on the Fe content)

 Iron Content (Fe) Maximum: 145g/L

 Pickle Agitation preferable

2.3 Analysis Procedures for the Acid Pickle

Acid strength and iron content should be checked frequently (frequency is dependent on throughput and tank
capacity). The analysis methods are outlined here;

1. Hydrochloric acid content (Section 2.3.1).

2. Iron content by titration (Section 2.3.2).
3. Iron content by the nomographic method (Section 2.3.3).

2.3.1 Hydrochloric Acid Content

Equipment Required

-100mL measuring cylinder

-25mL burette
-250mL conical flask
-adjustable pipettor (adjust to 2mL)
-100mL plastic bottle with a screw top lid

Reagents Required (see preparation of these in Appendix 2)

-1L 0.548N sodium bicarbonate

-100mL bromocresol green indicator

Method

1 Take a sample of about 100mL from the pickling bath in a plastic bottle and allow it to stand to cool to room
temperature and settle any sediment.
2 Using the clean pipettor, take 2mL of solution from the sample and transfer to the clean conical flask, and add
about 100mL of water.
3 To this solution add a few drops of bromocresol green indicator. The solution will turn yellow.
4 Fill the clean burette to the zero mark with 0.548N sodium bicarbonate and titrate slowly with the above
solution, while swirling the flask, until the solution turns permanent blue/green.
5 Record the burette reading. This is the endpoint (Titration, C).

Calculation
Titration, C, gives a direct measure of the hydrochloric acid content in the bath as percent weight per volume, ie. %
w/v. HCl % w/v = C To convert this to grams/litre; HCl g/L = C x 10

Example

If the endpoint of the HCl titration is 12mL, then HCl = 12% w/v OR HCl g/L = 12 x 10 = 120g/L

2.3.2 Iron Content in the Acid Pickle (Titration Method)

Equipment Required

-250mL measuring cylinder with a stopper

-100mL measuring cylinder
-25mL burette
-250mL conical flask
-adjustable pipettor (adjust to 10mL)
-small plastic funnel
-box of No.1 Whatman filter papers
-100mL plastic bottle with a screw top lid

Reagents Required (see preparation of these in Appendix 2)

1L 0.02M potassium permanganate

1L Zimmermann-Reinhardt reagent

Method

1 Take a sample of about 100mL from the pickling bath in a plastic bottle and allow it to stand to cool to
room temperature and settle any sediment.
2 Filter some of this sample into clean 25mL measuring cylinder to the 25mL mark exactly.
3 Pour this sample into clean 250mL measuring cylinder and make up to 250mL mark exactly with water.
Stopper the measuring cylinder and invert several times.
4 Using the clean pipettor, dispense 10mL of this dilute solution into the clean conical flask and add 15mL of
Zimmermann-Reinhardt reagent
5 Fill the clean burette to the zero mark with 0.02M potassium permanganate and titrate slowly with the
above solution, while swirling the conical flask, until the colour turns permanent pale pink.
6 Record the burette reading. This is the endpoint (Titration, D).

Calculation

Where D is the titration endpoint, the iron content of the acid pickle is calculated as follows; Fe g/L = D x 5.6

Example

If the endpoint from the iron titration is 10mL, then Fe g/L = 10 x 5.6 = 56 g/L

2.3.3 Iron content in the Acid Pickle (Nomographic Method)

Alternatively, iron content can be determined by the nomographic method. The nomograph is shown on the
following page.
Equipment Required

-Hydrometer for Specific Gravity (density range 1000 to 1200, with 0005 subdivisions)
-100mL measuring cylinder
-nomograph
-30cm ruler

Method

1 Take a 100mL sample from the pickling bath and allow it to stand to cool to room temperature and settle
any sediment.
2 Pour about 60-70mL of the clear sample into the clean measuring cylinder.
3 Place the hydrometer in the measuring cylinder and spin it to eliminate surface tension effects.
4 Read off the specific gravity (S.G.) at the fluid line.
5 Record the specific gravity of the flux sample.
6 Determine the HCl concentration by the method described previously.
7 Get a ruler and line up the “Specific Gravity (Density)” on the left-hand side of the graph with the
“Hydrochloric Acid Content” on the right-hand side of the graph.
8 The “Iron Content” can be read off the middle column where the line intersects the column.

Example

If the specific gravity was measured to be 1.165 and the HCl content was determined to be 115g/L (11.5% w/v),
then the line between the two outer columns intersects the middle column at Fe content = 55 g/L

See NOMOGRAPH BELOW

NOMOGRAPHIC METHOD Determination of Iron in Hydrochloric Acid

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3 PREFLUX
3.1 Introductory Comments

The purpose of the preflux is to provide a protective layer on the steel surface to prevent oxidation prior to
galvanizing and to break down the zinc oxide layer on the molten zinc surface at the point of entry of the steel into
the galvanizing bath. These conditions are critical to achieving a metallurgical reaction between the molten zinc
and the steel surface.

The following information refers specifically to preflux solutions consisting of zinc ammonium chloride (ZAC) “triple
salt” dissolved in water. Zinc ammonium chloride “triple salt” is the most commonly used form of preflux and has
the formula ZnCl2.3NH4Cl. The components are zinc chloride (ZnCl2) and ammonium chloride (NH4Cl) in the ratio
46% : 54% by weight, respectively.

Important parameters influencing flux performance and which must be monitored are:

i. Zinc ammonium chloride (ZAC) concentration

A concentration of 23 - 34% by weight is normally used. Measurement of the preflux density will give an
approximate indication of the ZAC concentration. Usually, density is measured as either Specific Gravity
 (S.G.) or ºBaumé (Bé). The graph below shows the relationship between these density measurements
and ZAC concentration. It should again be stressed that density measurements provide only an
approximation of ZAC concentration in that significant departures from the optimum ratio (refer below)
can introduce some error.

ii. Zinc chloride to ammonium chloride ratio

The ratio in the preflux solution should be maintained in the proportions similar to that in the solid crystal
form, ie. 46%ZnCl2 : 54%NH4Cl. During operation, the ratio can change and accordingly, adjustments may
be required from time to time to restore the ratio. Relatively small departures from the optimum ratio do
not have any detrimental consequences, however, if the ratio imbalance becomes excessive some adverse
effects can be experienced

In order to determine the ratio, measurement must be made of the individual components of the ZAC
solution, ie. Zinc content, ammonia content and chloride content. Procedures for analysing these are
given below.

(iii) Iron (Fe) content.

During operation of the preflux, the solution becomes contaminated with iron. The major sources of iron
are:

• Reaction of the preflux with the surface of the steel articles.

• Carry-over of iron salts on the surface of the steel articles from the acid pickle (water rinsing after
the acid pickle removes most but not all of the iron salts).

This iron contamination in the preflux will be transferred on the steelwork into the galvanizing zinc bath,
resulting in increased dross production. It is therefore very important in that the preflux be routinely
measured and that steps be taken to reduce this contamination to a minimum. It is generally accepted
that the iron content should not exceed 10g/L and through good practice many galvanizers are able to
achieve less than 5g/L.

It is important to note that iron in the preflux exists in two forms:

 Insoluble iron hydroxide. This form is responsible for the orange-brown colouration of the preflux
solution after it has been in use for a period of time. Most of this settles as a sludge in the bottom
of the tank and therefore does not present a major problem in the galvanizing process. This sludge
must be removed periodically otherwise it will be carried over into the galvanizing bath.
 Soluble iron chloride. Typically, in the preflux solution, the soluble iron content far exceeds the
insoluble form and it is the soluble iron which is therefore of greatest concern. Besides causing
increased dross production during galvanizing, it also reduces the effectiveness of the preflux to
chemically clean the steel surface.

Optimum operation of the preflux tank requires, firstly, that water rinsing after pickling is carried out as effectively
as possible to minimise iron salt carry over and, secondly, that as much of the soluble iron in the preflux solution is
converted to insoluble iron hydroxide. To achieve this conversion, the following procedures are commonly used;

a) Control of the preflux pH between 4.0 – 4.2 with 4.5 maximum. If preflux pH falls below 3.5 , insoluble
iron hydroxide will tend to reconvert to soluble iron. Solutions with pH values less than 4.0 can be
best adjusted to the optimum range (pH 4.0 – 4.2) by addition of ammonium hydroxide solution
(NH4OH).
b) Oxidation of the soluble iron content by either continuous air sparging of the preflux solution or by
hydrogen peroxide treatment (refer Section 3.6).

iv. pH of the preflux solution

As indicated above pH should preferably be maintained in the range 4.0 – 4.2 with 4.5 maximum. The
importance of the 4.0 minimum has been discussed above. Above 5.5 , zinc chloride will precipitate from
 solution as zinc hydroxide and is therefore not available for prefluxing the steel. Usually, preflux solutions
stabilize under normal operating conditions below pH 5.5; however if the pH should exceed 5.5 the preflux
solution can be adjusted back to the optimum range by addition of hydrochloric acid.

3.2 Summary of Recommended Operating Conditions for the Preflux

 Temperature Working Range: 55 - 65ºC (to facilitate drying of the steel prior to galvanizing)

 Zinc Ammonium Chloride Concentration (ZAC) Optimum Concentration: 230g/L – 340g/L

 Zinc Chloride to Ammonium Chloride Ratio Optimum Ratio: 46%ZnCl2 : 54%NH4Cl

 Iron Content (Fe) Maximum: 5 g/L

 Density measured at room temperature Working Range: 1.100 – 1.150 Specific Gravity (S.G.)

13.2 – 18.9º Baumé (Bé)

 pH Working Range: 4.0 – 4.2 with 4.5 maximum

3.3 Analysis Procedures for the Preflux

A full analysis of the preflux is recommended on a monthly basis. Measurement of density, pH and iron content
should be done more frequently (eg. weekly) and adjustments made as appropriate. The analysis procedures are
outlined in the following pages and include:

1. Iron content (section 3.3.1)

2. Zinc chloride content ( section 3.3.2)
3. Ammonium chloride content (section 3.3.3)
4. Total chloride content (section 3.3.4)
5. Various density measurement information ( 3.3 .5 – 3.3.8)
6. pH measurement (section 3.3.9)

3.3.1 Iron Content in the Preflux

Equipment Required

-250mL measuring cylinder with a stopper

. 25mL measuring cylinder
. 25mL burette

-250mL conical flask

-adjustable pipettor (adjust to 10mL)
-small plastic funnel
-Box of No.41 Whatman filter papers
-100mL plastic bottle with a screw top lid

Reagents Required (see preparation of these in Appendix 2)

. 1L 0.02M potassium permanganate

. 1L Zimmermann-Reinhardt reagent
Method

1 Take a sample of about 100mL from the preflux bath in a plastic bottle and allow it to stand to cool to
room temperature and settle any sediment.
2 Filter some of this sample into clean 25mL measuring cylinder to the 25mL mark exactly.
3 Pour this sample into clean 250mL measuring cylinder and make up to 250mL mark exactly with water.
Stopper the measuring cylinder and invert several times.
4 Using the clean pipettor, dispense 10mL of this dilute solution into the clean conical flask and add 15mL of
Zimmermann-Reinhardt reagent.
5 Fill the clean burette to the zero mark with 0.02M potassium permanganate and titrate slowly with the
above solution, while swirling the conical flask, until the colour turns permanent pale pink.
6 Record the burette reading. This is the endpoint (Titration, E).

Calculation

Where E is the titration endpoint, the iron content of the preflux is calculated as follows; Fe g/L = E x 5.6

Example

If the endpoint from the iron titration is 1.7mL, then Fe

g/L = 1.7 x 5.6 = 9.5 g/L

3.3.2 Zinc Chloride Content in the Preflux

Equipment Required

-1L volumetric flask, Morbank

-150mL beaker
-25mL measuring cylinder
-50mL burette
-250mL conical flask
-adjustable pipettor (adjust to 10mL)
-small plastic funnel
-box of No.41 Whatman filter papers
-100mL plastic bottle with a screw top lid

Reagents Required (see preparation of these in Appendix 2)

-1L 0.01M EDTA solution

-500mL 30% hydrogen peroxide
1L hydrochloric acid, technical (30% w/v)
1L buffer solution (pH – 10)

-100mL Erichrome black T (Erio T) indicator

Method

(CAUTION: Perform this determination in a well-ventilated room or fume cupboard because of ammonia fumes)

1 Take a sample of about 100mL from the preflux bath in a plastic bottle and allow it to stand to cool to
room temperature and settle any sediment.
2 Using the clean pipettor, take 10mL of solution from the sample and add to the clean volumetric flask, and
add water to the 1L mark exactly.
3 To this solution add about 2mL of the hydrochloric acid, stopper the volumetric flask and invert several
 times.
4 Using the clean pipettor, measure a 10mL sample from this dilute solution into the clean beaker, add a few
drops of hydrogen peroxide and about 10mL of the buffer solution. (NOTE: The solution will have an orange-
brown iron precipitate floating in it. This is normal and there is no need for concern).
5 The solution will need to be filtered through a No.41 paper into the clean conical flask to remove the iron.
After the solution has filtered through, rinse with water through the filter paper a few times into the flask.
6 To the filtered solution add a few drops of Erio T indicator and swirl the flask until the indicator mixes. The
solution will turn dark red.
7 Fill the clean burette to the zero mark with 0.01M EDTA solution and titrate slowly with the above
solution, while swirling the conical flask, until the colour turns permanent dark blue/green.
8 Record the burette reading. This is the endpoint (Titration, F).

Calculation

Where F is the titration endpoint, the zinc content of the preflux is calculated as follows; Zn g/L = F x 6.538 To convert this

to zinc chloride ZnCl2, ZnCl2 g/L = Zn g/L x 2.08

Example

If the endpoint from the zinc titration is 10mL, then Zn g/L = 10 x 6.538 = 65.4 g/L To convert this to zinc chloride, ZnCl2,

ZnCl2 g/L = 65.4 x 2.08 = 136 g/L

Quality Check

Using the above method, check the accuracy of the results with the standard preflux solution. Preparation of this
standard solution is outlined in Appendix 3

3.3.3 Ammonium Chloride Content in the Preflux

Equipment Required

-250mL measuring cylinder

-100mL measuring cylinder
-150mL beaker
-50mL burette
-250mL conical flask
-adjustable pipettor (adjust to 1mL)
-100mL plastic bottle with a screw top lid
-distillation apparatus (see Appendix 1)

Reagents Required (see preparation of these in Appendix 2)

1L 0.1N sulphuric acid

1L 0.1N sodium hydroxide
1L 40% sodium hydroxide

-100mL methyl red indicator

Method

(CAUTION: Perform distillation behind a Perspex screen or in a fume cupboard because of a possible explosion
from an acid-base reaction).
1 Set up the distillation apparatus as per diagram.
2 To the clean 150mL beaker (collection vessel), add exactly 50.0mL of the 0.1N sulphuric acid, then add a
few drops of the methyl red indicator. The solution will turn dark pink.
3 Place this collection vessel below the condenser tip of the distillation apparatus. Make sure the tip is
immersed in the acid solution.
4 Take a sample of about 100mL from the preflux bath in a plastic bottle and allow it to stand to cool to
room temperature and settle any sediment.
5 Using a clean pipettor, add 1mL of solution from the sample to the clean distillation flask with about
150mL of water.
6 To this solution add 50mL of the 40% sodium hydroxide. Seal the flask immediately with the glass stopper
as the reaction of releasing ammonia take place immediately.
7 When the distillation is fully set up turn water on at a moderate rate so that it flows through the
condenser tube continuously during the distillation.
8 Heat the contents in the distillation flask with a Bunsen burner until boiling occurs. Then lessen the heat,
continue to boil for 10 minutes and collect the distillate in the collection vessel.
9 When distillation has finished (after about 10 minutes);

i. Remove the collection vessel from under the condenser tip,

ii. Then turn off the Bunsen burner and the water.

(CAUTION: It is important to do this step in this precise order to prevent the distillate being sucked back into the
distillation flask and causing an EXPLOSION from the resultant acid-base reaction).
 1. Empty contents of collection vessel into the clean conical flask.
2. Fill the clean burette to the zero mark with 0.1N sodium hydroxide and titrate slowly with the above solution,
while swirling the conical flask, until the colour turns permanent yellow.
3. Record the burette reading. This is the endpoint (Titration,G).

Calculation
+
Where G is the titration endpoint, the ammonia content of the preflux is calculated as follows; NH4 g/L = (50.0 – G) x 1.8
+
To convert this to ammonium chloride, NH4Cl, NH4Cl g/L = NH4 g/L x 2.96

Example

If the endpoint from the ammonia titration is 20mL, then

+
NH4 g/L = (50.0 – 20) x 1.8 = (30) x 1.8 = 54 g/L

To convert this to ammonium chloride, NH4Cl, NH4Cl g/L = 54 x 2.96 = 160 g/L

Quality Check

Using the above method, check the accuracy of the results with the standard preflux solution. Preparation of this
standard solution is outlined in Appendix 3

3.3.4 Chloride Content in the Preflux

Comment: Determination of chloride content is a useful cross-check procedure, ie, it cross-checks the accuracy of
the zinc chloride and ammonium chloride measurements. Total chloride content as-measured should not
substantially differ from the combined chloride contents in the zinc chloride and ammonium chloride
determination. Refer to the example below.

Equipment Required

-100mL measuring cylinder with a stopper

-50mL burette
-250mL conical flask
-adjustable pipettor (adjust to 1mL for Step 2, then adjust to 10mL for Step 3)
-100mL plastic bottle with a screw top lid

Reagents Required (see preparation of these in Appendix 2)

-1L 0.1N silver nitrate

-100mL potassium chromate indicator
-20L distilled water (IMPORTANT: Water should have no chloride present to affect the result)

Method

1 Take a sample of about 100mL from the preflux bath in a plastic bottle and allow it to stand to cool to
room temperature and settle any sediment.
2 Using the clean pipettor, take 1mL of solution from the sample and transfer it to the clean 100mL
measuring cylinder and make up to the 100mL mark with distilled water. Stopper the measuring cylinder and
invert several times.
3 Using the clean pipettor, measure 10mL of this dilute solution into a clean conical flask and add about
100mL of distilled water.
4 To this solution, add a few drops of the potassium chromate indicator. The solution will turn bright yellow.
 5 Fill the clean burette to the zero mark with 0.1N silver nitrate and titrate slowly with the above solution,
while swirling the conical flask, until the colour turns permanent orange/brown.
6 Record the burette reading. This is the endpoint (Titration, H).

Calculation

Where H is the titration endpoint, the chloride content of the preflux is calculated as follows; Cl

g/L = H x 35.46

Example

If the endpoint of the chloride titration is 5.0 mL, then Cl g/L = 5.1 x 35.46 = 177 g/L

Cross-check with ZnCl2 and NH4Cl Determinations

Chloride component of Zinc Chloride Where x is the chloride component in zinc chloride, the following formula is
used to calculate the chloride contribution; x = Zn g/L x 1.09

Chloride component of Ammonium Chloride Where y is the chloride in ammonium chloride, the following formula
+
is used to calculate the chloride contribution; y = NH4 g/L x 1.97

Total Chloride The total chloride is the sum of the chloride components in zinc chloride and ammonium chloride.

Total Cl g/L = x + y

3.3.5 Density Measurement of the Preflux

Density of the flux solution at room temperature is a quick but only approximate indication of ZAC concentration.
The following page shows a graph of ZAC concentration versus density, expressed as specific gravity (S.G.), at room
temperature. A table converting density, in g/mL, to ºBaumé (Bé) is also provided later.

Equipment Required

-Hydrometer for Specific Gravity (density range 1000 to 1200, with 0005 subdivisions)
-100mL measuring cylinder

Method

1 Take a 100mL sample from the preflux bath and allow it to stand to cool to room temperature and settle
any sediment.
2 Pour about 60-70mL of the clear sample into the clean measuring cylinder.
3 Place the hydrometer in the measuring cylinder and spin it to eliminate surface tension effects.
4 Read off the specific gravity (S.G.) at the fluid line.

4. Record the specific gravity of the preflux sample. (See schematic diagram and photograph of specific

gravity measurement later).

For example, the S.G. figure read from the hydrometer is 1170, the true representation of S.G. is 1.170.
3.3.6 ZAC Concentration vs S.G. at room temperature

ZAC Concentration vs Specific gravity graph

3.3.7 Conversion of Density to Baumé

There is formula which can be used to convert density in g/mL to ºBaumé (Bé) and vice versa. This is shown
below:

Where the density is known and the ºBaumé scale is required the following formula can be used;
Bé = ºBaumé Bé = 145 – (145) / d = density in g/mL

Example d = 1.10

3.3.8 MEASUREMENT OF SPECIFIC GRAVITY

This photograph and diagram demonstrate how the specific gravity of a particular bath sample is measured.
NOTE; S.G. is read off at the fluid line. In this example the density of the sample is 1170 which is expressed as S.G.
– 1.170.
3.3.9 pH measurement of the Preflux

The pH level of the preflux should be checked on a regular basis using a portable pH meter or pH indicator paper
test strips. The method for this is outlined below.

Equipment Required

a) A portable pH meter

OR

b) A box of pH indicator papers (The papers should cover the range pH 0 – pH 7 and be graduated in pH = 0.1
intervals).

Method

A. The pH meter needs to be calibrated before use. Refer to manufacturers recommendations in the
operating manual. Take a preflux sample of about 20mL and allow to cool to room temperature, place the
tip of the pH meter in the sample and read off the pH on the digital display.
(IMPORTANT: Rinse the tip of pH meter in water and wipe the tip between samples).

OR alternatively,
 A. Take a preflux sample of about 20mL and allow to cool to room temperature. Take a test strip, dip it in the
quench sample for a few seconds and upon removal, compare the colours on the test strip to the colour
chart on the box.

3.4 Iron Control Procedures for the Preflux

Iron is present in the preflux in two forms: an insoluble iron hydroxide (which gives the solution its familiar orange-
brown colour) and a soluble iron chloride. Typically, the soluble iron content far exceeds the insoluble form and it
is the soluble iron which is therefore of greatest concern.

Excessive (>5 g/L) iron in the preflux impedes fluxing action and results in increased dross production. Removal of
soluble iron from the preflux may be done in several ways, as follows:

i. Air Sparging

This method is very slow as it requires the bubbling of air through the preflux for an extended period. The
pH of the preflux must be maintained between 4.0-4.5 to prevent iron converting back to the soluble
form.

Air sparging is carried out on a continuous basis in the operating tank. The operation is not efficient, as
only a portion of the soluble iron is oxidised and it results in disruption to the process.

ii. Hydrogen Peroxide Oxidation

This is a far more effective method and involves the addition of hydrogen peroxide to the preflux in order
to rapidly oxidise the soluble iron to the insoluble (hydroxide) form.

Traditionally, the operation is done as a batch process, ie, the preflux is pumped into a spare tank and
treated. The insoluble iron is then allowed to settle which can take a considerable period of time. The
clear solution is eventually pumped back to the operating preflux tank.

As an alternative, peroxide can be added to the operating tank on a semi-continuous basis.

In both cases, as the addition of hydrogen peroxide lowers the pH, regular additions of ammonium
hydroxide (not to be confused with ammonium chloride) are required to ensure that pH is maintained
between 4.0-4.5. The pH of the preflux should be monitored throughout the process so that the
appropriate additions of ammonium hydroxide can be made. If the pH of the preflux is allowed to drop
below pH 4.0, the oxidised iron will begin to convert back to the soluble form. It is therefore strongly
advised that the hydrogen peroxide is not all added at once but instead, progressive separate additions
are made, with a pH check after each addition and pH adjustment with ammonium hydroxide if
necessary.

The amount of hydrogen peroxide (H2O2) required depends on H2O2 strength, iron content and the
volume of the bath. As a guide, one litre of 30% H202 is required for every 1300 grams of iron in the
preflux.

Example:

A 20 000 litre preflux with an iron content of 35 g/L. To reduce iron content to say 5 g/L, H2O2
required;

20 000 litres x 30 g/L = 600 000 grams of iron;

600 000/1300 = 460 litres.

Therefore approximately 460 litres of H2O2 are required to reduce iron in the preflux from 35 g/L to 5 g/L.
Normally double the amount (920 litres) of ammonium hydroxide is required for pH corrections.
The level of iron in a preflux can normally be maintained below 10 g/L by paying careful attention to pH
 control and iron carry-over from the acid pickle. The pH of the preflux should be monitored regularly to
prevent it falling below 4.5. Adjustments can be made by using ammonium hydroxide. Efficient rinsing after
acid pickling will prevent an excessive iron carry-over to the preflux.

After treatment has been completed, the preflux liquor strength needs to be checked and any appropriate
adjustments made.

WARNING - Hydrogen peroxide and ammonium hydroxide are dangerous chemicals and require careful
handling with all appropriate safety equipment.

iii. CEPT Technology

The Industrial Galvanizers Corporation (IGC) have developed a continuous method of removing soluble iron
from flux solutions. The Continuous Electrolytic Preflux Treatment (CEPT) electrolytically oxidises soluble
iron to produce a dense, insoluble form that has rapid settling characteristics.

IGC claims that the system will maintain soluble iron level below 1 g/L and because the system is continuous,
there is no loss of plant operating time.

4 QUENCH – PASSIVATION (Sodium Dichromate Solution)

4.1 Introductory Comments

The quench has two functions. The primary function is to cool the freshly galvanized articles to a temperature
suitable for subsequent handling. The other function of the quench is, where sodium dichromate
(Na2Cr2O7.2H2O) is intentionally added to the water, to apply a thin chromate conversion coating to the
galvanized coating to prevent white rusting. This is termed chromate passivation.

The three main factors controlling the effectiveness of passivation are;

i. The sodium dichromate concentration

Start-up fresh tank

A recent survey of several galvanizers by ZTS has shown 0.3 – 0.5 g/L to be an indicative sodium
dichromate (anhydrous) concentration for start-up (fresh tank). This is equivalent to a chromium
content of 120 – 200 mg/L (ppm).

To ensure rapid and full dissolution of the chromate, dissolve it into a quantity of hot water
(>70°C) prior to addition to the tank. After one week of operation, increase the chromate
progressively to the “working tank” levels below.

Working tank

A recent of several galvanizers by ZTS has shown 0.8 – 1.5 g/L to be an indicative sodium
dichromate (anhydrous) concentration for a working tank of quench water. At this concentration,
the level of free chromium will be 320 – 480 mg/L (ppm).

Higher concentration solutions may discolour the galvanized coating whilst lower concentration
solutions may not provide sufficient passivation. The concentration may be adjusted by adding
sodium dichromate or water to the bath.
 These are indicative levels only and individual galvanisers may need to alter sodium dichromate
concentrations depending on the thickness of work or the atmospheric conditions.

ii. The pH of the quench

The pH of the solution is also important as the passivation process requires a slightly acidic solution. The
quench pH should be maintained between 5.0 - 6.5 and sulphuric acid can be used to bring pH down to the
desired level.

iii. Chloride (Cl) content

The chloride content is a function of ash/flux carry-over from the galvanizing bath. Chloride level should
be maintained below 0.1% or 1 g/L.

Although zinc is present in the quench from jigs and galvanized articles, it is not considered a problem.

4.2 Summary of Recommended Operating Conditions for the Quench

Temperature Working Range: 60-70ºC

Sodium Dichromate (anhydrous) Concentration (Na2Cr2O7)

Start up (fresh tank) 0.3 – 0.5 g/L ( = 0.03 – 0.05% chromate concentration)

Working Range: 0.8 – 1.2 g/L ( = 0.08 – 0.12% chromate concentration)

Very thick steel sections can develop a greenish colouration at these chromate levels. If plant throughput contains
a substantial proportion of thicker sections, reducing the chromate to 0.1% or marginally less should be
considered.

Chromium Content (Cr ) Start-up (fresh tank) 120 - 200 mg/L Working Range: 320 - 480 mg/L

(for the above concentration of sodium dichromate).

Chloride Content (Cl) Maximum: 1 g/L (0.1%) max

pH Working Range: 5.0 - 6.5

4.3 Analysis Procedures for the Quench

A full analysis of the quench should be done on a monthly basis. The methods of analysis are outlined over the
page which include:

1. Chromium content (Section 4.3.1).

2. Chloride content (Section (4.3.2).
3. pH measurement (Section (4.3.3).
4.3.1 Chromium Content in the Quench

Equipment Required

. 25mL measuring cylinder

. 25mL burette

-adjustable pipettor (adjust to 10mL)

-100mL plastic bottle with a screw top lid
-a teaspoon

Reagents Required (see preparation of these in Appendix 2)

. 1L 0.1N sodium thiosulphate

. 1L 10% sulphuric acid

-500g solid potassium iodide

-100mL starch solution (VITEX) indicator

Method

1 Take a sample of about 100mL from the quench bath in a plastic bottle and allow it to stand to cool to
room temperature and settle any sediment.
2 Using a clean pipettor, measure 10mL of the sample into the clean conical flask, and add 20mL of sulphuric
acid.
3 To this solution add 2g (about half a teaspoon) of potassium iodide. The solution will turn yellow through
to red/brown depending on the chromate content. Stir vigorously for 5 minutes.
4 Add a few drops of starch (VITEX) indicator. The solution will turn dark brown/black.
5 Fill the clean burette to the zero mark with 0.1N sodium thiosulphate and titrate slowly with the above
solution, while swirling the conical flask, until the black colour turns clear.
6 Record the burette reading. This is the endpoint (Titration, J).

Calculation

Where J is the titration endpoint, the chromium content of the quench is calculated as follows; Cr mg/L = J x 173.4

Example

If the endpoint of the chromium titration is 3mL,

then Cr mg/L = 3 x 173.4 = 520.2 mg/L

4.3.2 Chloride Content in the Quench

Equipment Required

-100mL measuring cylinder

-25mL burette
-250mL conical flask
-adjustable pipettor (adjust to 5mL)
-100mL plastic bottle with a screw top lid

Reagents Required (see preparation of these in Appendix 2, page 57)

 -1L 0.1N silver nitrate
-100mL potassium chromate indicator
-20L distilled water (IMPORTANT: Water should have no chloride present to affect the result)

Method

1 Take a sample of about 100mL from the quench bath in a plastic bottle and allow it to stand to cool to
room temperature and settle any sediment.
2 Using the clean pipettor, measure 5mL of the sample into the clean conical flask and add about 100mL of
distilled water.
3 To this solution, add the potassium chromate indicator. The solution will turn bright yellow.
4 Fill the clean burette to the zero mark with 0.1N silver nitrate and titrate slowly with the above solution,
while swirling the conical flask, until the colour turns permanent orange/brown.
5 Record the burette reading. This is the endpoint (Titration, K).

Calculation

Where K is the titration endpoint, the chloride content of the quench is calculated as follows; Cl g/L = K x 0.7092

Example

If the endpoint of the chloride titration is 3mL,

then Cl g/L = 3 x 0.7092 = 2.1 g/L

4.3.3 pH Measurement of the Quench

The pH level of the quench should be checked on a regular basis using a portable pH meter or pH indicator paper
test strips. The method for this is outlined below.

Equipment Required

a) A portable pH meter

OR

b) A box of pH indicator papers (The papers should cover the range pH 0 – pH 7 and be graduated in pH = 0.1
intervals)

Method

a. The pH meter needs to be calibrated before use. Refer to manufacturers recommendations in the operating
manual. Take a quench sample of about 20mL and allow to cool to room temperature, place the tip of the
pH meter in the sample and read off the pH on the digital display. (IMPORTANT: Rinse the tip of pH meter
in water and wipe the tip between samples).

OR alternatively,

b. Take a quench sample of about 20mL and allow to cool to room temperature. Take a test strip, dip it in the
quench sample for a few seconds and upon removal, compare the colours on the test strip to the colour
chart on the box.
6 APPENDIX 1 - Facilities and Equipment
6.1 Facilities Required

Preferably analysis of process liquors should be done in a dedicated room around 3m x 3m in size. If this is not
available, alternatively, the equipment can be stored in cupboards and used as required. The following facilities
are required, in either situation;

-running water with a sink.

-electricity for lighting and power.
-gas supply either on-line or bottle for the Bunsen burner.
-air conditioning to maintain a clean environment.

6.1.1 Laboratory Equipment Required

-50mL (PMP or TPX) plastic beaker

-150mL (PMP or TPX) plastic beaker
-1L (PMP or TPX) plastic volumetric flask, Morbank
-250mL measuring cylinder with a stopper
-100mL measuring cylinder with a stopper
-25mL measuring cylinder
-0-10mL adjustable pipettor
-dropper
-teaspoon
-small plastic funnel
-250mL plastic wash bottle
-100mL plastic bottles with screw top lid (to collect liquor samples in, x 100)
-a box of No.41 Whatman filter papers
-hydrometer (density range 1000-1200, 0005 graduations)
-portable pH meter or pH indicator papers (pH – 0.1 intervals)
-measuring balance (optional) – (necessary when preparing own reagents, indicators and standard solutions).
Able to measure up to 150g and be accurate to 0.01g.
-titration apparatus (see pages 22-24 for set up details)
-distillation apparatus (see pages 25-27 for set up details)
-perspex screen or fume cupboard with a sink and running water for distillation

Note: PMP and TPX are special high temperature, high clarity plastics.

6.1.2 Safety Equipment

-safety glasses
-rubber gloves
-leather shoes
-laboratory coat (optional)
-face shield (optional)
-safety shower and eyewash station

6.2 Titration Equipment

A schematic diagram, is shown below, along with a photograph of the set on the following page.

Equipment Required
 burette clamp
burette stand

-50mL (PMP or TPX) plastic burette

-25mL (PMP or TPX) plastic burette
-250mL (PMP or TPX) plastic conical flask

Titration apparatus
6.2.1 TITRATION APPARATUS

This photograph shows the typical set up for the titration apparatus.

6.3 Distillation Equipment

A schematic diagram along with a photograph of the set up is included on the following pages.

Equipment Required

-1 x Bunsen burner (with gas supply)

2 x Bossheads
 2 x clamps

1 x stand
1 x 150mL beaker
1 x 250mL round bottom flask, two necks: (side neck at 20º angle, socket size 19/24) (centre neck socket
size 24/29)

-
1 x glass stopper: (cone size 19/24) -
1 x splash head condenser, straight: (cone size 24/29) (socket size 19/26)

-
-1 x condenser tube (Leibig): (socket size 24/29) (jacket length 250mm)

-2 x adapters: cone to nozzle, without stopcock:

1 to fit splash head, angled nozzle 90º - (cone size 19/26) (angled nozzle 8mm OD)

1 to fit condenser tube, straight nozzle - (cone size 24/29) (straight nozzle 8mm OD)
-2 x 0.5m PVC plastic tubing: 1 for cold water from tap to condenser inlet (8mm ID). 1 for cold water from
condenser outlet to sink (8mm ID).

-1 x 0.5m high temperature plastic tubing: join splash head adapter nozzle with condenser tube adapter
nozzle (8mm ID).

IMPORTANT: For safety reasons the distillation will need to be performed in a fume cupboard or behind a Perspex
screen.

A sink and running water in the fume cupboard is preferred.

6.3.1 DISTILLATION APPARATUS (Analysis of Ammonia in Preflux Solution)

This photograph shows the general set up of the distillation apparatus.

7 APPENDIX 2 -Reagents and Indicators

Reagents Required

Available as “off the shelf” Reagents

-1L 0.1 N hydrochloric acid

-2.5L hydrochloric acid, technical (30% w/v)
-500mL 30% hydrogen peroxide
-500g potassium iodide
1L 0.02M potassium permanganate
1L 0.1N silver nitrate
1L 0.1N sodium hydroxide
1L 0.1N sodium thiosulphate
1L 0.1N sulphuric acid
1L 10% w/w sulphuric acid

Reagents to be Prepared (see details of preparation later)

1L buffer solution (pH – 10)

1L 0.01M EDTA solution
1L 0.548N sodium bicarbonate
1L 40% sodium hydroxide
1L Zimmermann-Reinhardt reagent

Indicators Required (see details of preparation listed later)

100mL bromocresol green indicator

100mL eriochrome black T (Erio T) indicator
100mL methyl red indicator
100mL phenolphthalein indicator
100mL potassium chromate indicator
100mL starch solution (VITEX)

Other Chemicals Required (for preparation of reagents and indicators)

-500g ammonium chloride

-2.5L ammonium hydroxide
-20L distilled water
-2.5L ethanol
-500g magnesium sulphate, hydrated
2.5L 85% phosphoric acid
2.5L 98% sulphuric acid
2.5L triethanolamine

7.1 Preparation of Reagents and Indicators Reagents

Buffer solution (pH-10) – Weigh out 70g ammonium chloride, then dissolve in 568mL of ammonium hydroxide and
make up to the 1L mark exactly in a volumetric flask with distilled water.

0.01M EDTA solution – Dissolve 3.72g of A.R. disodium dihydrogen ethylenediaminetetra-acetate dihydrate (EDTA)
in distilled water and make up to the 1L mark exactly in a volumetric flask with distilled water.

0.548N Sodium Bicarbonate – Dissolve 46g of sodium bicarbonate in distilled water and make up to the 1L mark
exactly in a volumetric flask with distilled water.

40% Sodium Hydroxide – to 1L of water, cautiously add 40g of sodium hydroxide pellets and stir until dissolved.

Zimmermann-Reinhardt Reagent – Dissolve 70g of manganese sulphate in 500mL of water, cautiously add 125mL
(98%) sulphuric acid and 125mL (85%) phosphoric acid, make up to 1L mark exactly with water.
CAUTION: 40% sodium hydroxide solution and Zimmermann-Reinhardt reagent. (Preparation of these solutions
must be performed in a fume cupboard or behind a Perspex screen for safety reasons as an explosion can result).

Indicators

Bromocresol Green – generally available as “off the shelf” solution.

Dissolve 0.1 g of bromocresol green in 100mL of distilled water.

Eriochrome Black T (Erio T)

Dissolve 1g of eriochrome black T dyestuff in 75mL of triethanolamine and 25mL of ethanol.

Methyl Red – generally available as “off the shelf” solution.

Dissolve 0.1g of methyl red, water-soluble sodium salt, in 100mL of distilled water.

Phenolphthalein

Dissolve 0.5g of solid phenolphthalein in 50mL of absolute alcohol, then add 50mL of distilled water.

(Filter if necessary).

Potassium Chromate

Dissolve 5g of solid potassium chromate in 100mL of distilled water.

Starch Solution (VITEX)

Dissolve 1g of solid vitex indicator in 100mL of distilled water.

8 APPENDIX 3 Quality Check & Preparation of Standard Solutions

Equipment Required

500mL (PMP or TPX) plastic volumetric flasks

500mL (PMP or TPX) plastic beaker

-measuring balance
-250mL measuring cylinder

Reagents Required

-distilled water
-2.5L hydrochloric acid, technical (30% w/v)
500g iron (II) sulphate, heptahydrate (FeSO4.7H2O)
500g sodium chloride
500g sodium dichromate
500g sodium hydroxide pellets
500g sodium carbonate, anhydrous

-1L 10% w/w sulphuric acid

-500g zinc ammonium chloride (ZAC)

Preparation of Standard Solutions

Sodium hydroxide (Standard composition: NaOH – 80 g/L; Ratio – 0.9)

 Dissolve 40g of sodium hydroxide pellets along with 5g of sodium carbonate in about 150mL of distilled
water in a clean beaker. Transfer this solution to a clean volumetric flask and make up to the 500mL mark
exactly with distilled water. Stopper the flask and invert several times.

Acid (Standard composition: HCl – 120 g/L: Fe – 50 g/L)

Add 174mL of hydrochloric acid to about 150mL of distilled water in a clean beaker, then dissolve 125g of
iron sulphate. Transfer this solution to a clean volumetric flask and make up to the 500mL mark exactly
with distilled water. Stopper the flask and invert several times.
+
Preflux (Standard composition: Fe – 10 g/L; Zn – 65 g/L; NH4 - 55 g/L: Cl – 180 g/L)

Dissolve 150g of ZAC along with 25g of iron sulphate in about 150mL of distilled water in a clean beaker. In
addition, 10mL of sulphuric acid will need to be added to the solution to stop the iron oxidising to form a
precipitate. Transfer this solution to a clean volumetric flask and make up to the 500mL mark exactly with
distilled water. Stopper the flask and invert several times.

Quench (Standard composition: Cr – 500 mg/L; Cl – 2 g/L)

Dissolve 0.72g of sodium dichromate along with 1.64g of sodium chloride in 150mL of distilled water in a
clean beaker. Transfer this solution to a clean volumetric flask and make up to the 500mL mark exactly
with distilled water. Stopper the flask and invert several times.

Perform the analysis on each standard solution as per the relevant method described in Section 8.3 through to
Section 8.6.

Check the accuracy of your bath samples with those of your prepared solutions.

NOTE: The results from these standard solutions should be recorded as part of your Quality Assurance.