Turbidity Standards
Turbidity Standards
Turbidity Standards
C83
7045
Printed in U.S.A.
In memory of
Clifford C. Hach
(1919-1990)
inventor, mentor, leader and, foremost,
dedicated chemist
Introduction 4
Importance of Primary Standards
Definition of Primary Standard
Turbidity Standards
Standard Methods Clarification of Primary vs Secondary Standards
Primary Turbidity Standard Development5
Definition of Turbidity
Turbidity Units of Measure
Formazin as a Primary Turbidity Standard
Using Formazin Standards 7
Preparation of Formazin Stock Suspension
Preparation of Formazin Calibration Standards
Storage of Formazin Stock Suspensions
StablCal Stabilized Formazin Standards 8
Theory Behind Stability
Stability Data
Comparability
Secondary Standards 11
Application of Secondary Turbidity Standards
Latex Secondary Turbidity Standards
Gelex Secondary Turbidity Standards
Using Gelex Turbidity Standards
Care and Storage of Gelex Turbidity Standards
Alternative Standards 12
Definition of Alternative Standard
Application of Alternative Standards
Appendix I. Preparation of Formazin 12
Appendix II. Preparing Formazin Dilutions 13
Appendix III. Preparing StablCal Standards 13
Appendix IV. Using Low Range StablCal Standards for Verification of Calibration 15
Appendix V. Apparatus and Reagents 18
Introduction
Importance of Standards
All scientific work depends on precise measurement to
assure meaningful results. British mathematician and
physicist Lord Kelvin expressed the necessity of accurate
measurement over 100 years ago: If you can measure
that of which you speak, and you can express it in
number, you know something of your subject; but if
you cannot measure it, your knowledge is meager
and unsatisfactory.
Standards are the foundation of scientific measurement,
the fundamental units in which we describe our work.
They provide the terms we need to express conditions,
procedures, and results, serve as a reference against
which other measurements are compared, and establish
a basis for compatibility in communication of scientific
work throughout the world.
Turbidity Standards
The subject of standards in turbidimetric measurement
is complicated partly by the variety of types of standards
in common use and acceptable for reporting purposes
by organizations such as the USEPA1 and Standard
Methods, and partly by the terminology or definition
applied to them.
In the 19th edition of Standard Methods for the Examination
of Water and Wastewater, clarification was made in defining
primary versus secondary standards. Standard Methods
defines a primary standard as one that is prepared by the user
from traceable raw materials, using precise methodologies
and under controlled environmental conditions. In turbidity,
the only standard that can be defined as primary is formazin
that has been prepared by the user on the bench.
1United
Development of the
Primary Turbidity Standard
Glass
Sample Cell
Definition of Turbidity
Lamp
Transmitted
Light
Lens
90 Scattered
Light
Detector
Aperture
Incident
Beam
Size: Approximately 1/4 the
Wavelength of Light
Size: Smaller Than 1/10
the Wavelength of Light Description: Scattering Concentrated
Description: Symmetric in Forward Direction
Incident
Beam
Incident
Beam
N
H
(1)
N
+ 6H2O
(2)
n
2
(from hydrazine
sulfate)
Hexamethylenetetramine
H
+ 2H 2 SO 4
+ 2(NH 4 ) 2 SO 4
H
Formaldehyde
:N
N:
+ nH2O
Hydrazine
Formazin
StablCal Stabilized
Formazin Standards
Time in Days
Since The Standards
Were Prepared
0
8
16
24
31
41
55
65
73
84
94
105
120
133
141
233
369
478
576
602
671
716
734
827
2 NTU
Traditional
Formazin
2.03
1.95
1.94
1.80
2.02
1.66
1.64
1.62
1.70
1.46
1.27
1.35
1.03
0.88
0.75
0.39
0.58
0.05
0.27
0.13
0.09
0.08
0.08
0.07
2 NTU
StablCal
Formazin
1.96
1.96
1.95
1.96
1.96
1.97
1.96
1.95
1.97
1.92
1.96
1.94
1.93
1.93
1.94
1.90
1.91
1.96
1.96
1.96
1.93
1.91
1.95
1.95
2.50
2.00
1.50
2 NTU Traditional Formazin
2 NTU StablCal Formazin
1.00
0.50
0.00
0
100
200
300
400
500
600
700
800
Comparability:
Once the StablCal standards were demonstrated to be
stable, the next test was to determine and compare the
functional aspects of StablCal standards to traditional
prepared formazin standards.
Table 1: Instruments calibrated on traditional formazin. Both StablCal Stabilized Formazin Standards and
traditional formazin standards were read relative to traditional formazin. The results are displayed below:
Instrument 40 NTU
40 NTU
20 NTU
20 NTU
10 NTU
10 NTU
5 NTU
5 NTU
2 NTU
2 NTU
1 NTU
1 NTU
Make and StablCal Standard
StablCal Standard StablCal Standard StablCal Standard StablCal Standard StablCal Standard
Model Formazin Formazin Formazin Formazin Formazin Formazin Formazin Formazin Formazin Formazin Formazin Formazin
Hach
39.7
39.4
20.1
19.9
10.0
9.91
5.15
5.02
2.03
2.07
1.10
1.05
2100AN
(NonRatio
Mode)
Hach
40.0
40.3
19.7
19.9
9.78
10.1
4.94
5.00
1.97
2.06
1.07
1.03
2100AN
Ratio Mode
Hach
39.6
39.5
19.9
19.7
9.95
9.76
5.15
4.99
2.00
2.06
1.06
1.04
2100AN IS
NonRatio
Mode
Hach
39.8
40.3
19.7
19.7
9.80
9.89
5.03
4.98
1.97
2.06
1.06
1.03
2100AN IS
Ratio
Mode
Monitek
38.3
39.0
19.7
19.8
9.90
9.87
4.97
4.83
1.95
1.97
1.05
1.01
Model 21
LaMotte
41.0
40.4
20.0
20.0
10.1
10.1
4.78
5.00
2.00
2.04
0.96
1.00
Model
2008
Hach
41.5
39.6
20.0
19.5
9.95
10.0
5.00
5.12
2.20
2.15
1.10
1.08
2100A
Hach
39.0
40.3
19.4
19.8
9.70
10.1
4.94
5.04
1.97
2.08
1.09
1.07
2100P
10
Conclusion:
Secondary Standards
Definition of Secondary Standard
Primary standards may be prepared directly, and their
values are defined. The value of a secondary standard
is derived by reference to a primary standard. By
measuring against a primary standard, and in many cases
adjusting to match the primary, a secondary standard is
established as having a known value to be used for
subsequent comparisons.
In physical measurement, secondary standards are
required because there may be only one master standard
defined and accepted as the standard unit (e.g. kilogram),
and copies must be made for actual use. These
secondary standards are often referred to as transfer
standards, and are usually certified. Their derived value
is traceable to the original primary standard. It is
accepted that copies cannot be made to absolute perfection
and contain probability for error.
Alternative Standards
Definition of Alternative Standard
Appendix I. Preparation of
Primary Formazin
2. Dissolve 10.00 g of analytical grade hexamethylenetetramine, (CH2)6N4, in ultra-filtered deionized water and
dilute to 100 mL in a Class A, 100 mL volumetric flask.
12
Table 2
Desired NTU
Standard
2
4
6
10
20
40
100
200
mL of 1000 NTU
Suspension
0.2
0.4
0.6
1.0
2.0
4.0
10.0
20.0
Notes
A. Dilute formazin standards are stable only for a
short period of time, and should be used immediately
after preparation.
B. Use Hach prepared 4000 NTU Formazin Stock
Suspension, or prepare a 4000 NTU suspension
following the procedure in Appendix I.
For example, to prepare a 100 mL, 4 NTU suspension starting with a 1000
NTU working suspension, find the required amount of 1000 NTU suspension:
13
4. Wait 2 to 3 minutes.
5. Place the standard into the turbidimeter; record the
value or perform the calibration point measurement.
5. Fill the sample cell with the standard; cap the sample
cell and, if used, cap, the bulk sample.
14
Appendix IV. Using Low Range StablCal Standards for verification of calibration
(Standards between 0.10 and 1.0 NTU)
15
0.297 NTU
16
Troubleshooting
Process Instruments
If the process instrument reading is high, clean the
turbidimeter body and bubble trap again. Rinse
thoroughly with ultra-filtered deionized water. (Ultrafiltered water may be produced by filtering deionized
water through a 0.2-m filter or smaller. This water will
have a turbidity between 0.020 and 0.050 NTU.) Repeat
the test with fresh standard. The previously used
standard may have been contaminated from a dirty
turbidimeter body and should not be reused.
Notes
a. Use one of the following cleaning procedures for
sample cells. The first procedure involves filling the
sample cells with 1:1 hydrochloric acid. Cap the cells
and place them in a sonic bath for 5 minutes. Then,
allow the cells to stand for another 30 minutes. Follow
by rinsing both the cells and caps at least 10 times with
ultra-filtered deionized water. Immediately cap after
rinsing in order to prevent contamination. Dry the
outside surface of the capped cell with a soft cloth.
The second cleaning procedure involves scrubbing the
sample cells, both inside and out, with a mild laboratory
detergent (e.g., Liqui-nox Detergent), and a soft brush.
Immediately follow by rinsing at least 10 times with ultrafiltered water. Cap to prevent contamination. Dry the
outside surface of the capped cell with a soft cloth.
b. For process instruments, both the bubble trap and the
turbidimeter body must be thoroughly cleaned. Refer to
the cleaning instructions in the respective instrument
manual for details.
c. Once the StablCal Standard has been mixed, it has a
reading window of between 5 and 60 minutes, excluding
spikes. During this time, the standard does not need to
be re-mixed. The standard should be inverted between
3 to 5 times every hour to keep the formazin
polymer suspended.
17
Description
Hydrazine Sulfate, ACS grade
Hydrazine Sulfate, ACS grade
Hexamethylenetetramine, analytical grade
Volumetric Flask, 100 mL, Class A
Amber Bottle, Narrow Mouth, LPE, 250 mL, 6/pkg
Unit
20 g
100 g
500 g
each
each
500 mL
each
each
pkg
set
set
set
set
set
set
set
set
set
set
set
set
set
set
each
set
set
set
each
each
each
each
each
each
each
each
each
each
each
each
Or, in place of the 0.50 through 10.00 mL pipets, use TenSette Pipets:
19700-01
TenSette Pipet, 0.1 to 1.0 mL, 0.1 mL increments
19700-10
TenSette Pipet, 1.0 to 10.0 mL, 1.0 mL increments
each
each
18
set
set
set
set
set
set
set