Professional Documents
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183
Process
Sample
Hardware
Sample
Technique
Sample
Processing
Sample
Evaluation
The
consistency Errors Measured
consistency
‘Additives’ here typically means filler: China clay, titanium dioxide, calcium car-
bonate, talc or contaminants such as printing ink, etc. In the majority of cases,
there is no additive and in this case the total consistency = fiber consistency. The
proportion of non-flammable additives as above is calculated by means of an ‘ash
content test’.
184
Common ball valve as sampling valve
A ball valve is often used, as it is the cheapest in price. But it is usually a very un-
reliable solution if it is not handled in a very well-defined way each time a sample
is to be taken. Practical experience shows that different people open the valve dif-
ferently, which means that test results will vary considerably from case to case.
Also, such a standard valve takes the sample close to the pipe wall, where it is
most often not representative. More often than not, the pulp flows forwards in a
‘plug flow’, which means that a film of water forms close to the wall of the pipe.
This film of water (and the adjacent points where consistency gradually decreas-
es, approaching the water film) can reach a considerable thickness in many cases
(see Fig. 2.3). The ‘diluted area’ will therefore have a significant effect on the sam-
ple taken with such a valve – the apparent consistency sampled will be too low.
Not only that; if the valve is not fully open, de-watering will take place between
the ball and its seat, and the consistency of the sample will be too low for this rea-
son.
The higher the pipe pressure or the lower the consistency, the greater is the risk
of a further complication: if the valve is opened further, a large amount of pulp
will spray rapidly out at high pressure. The pulp will be difficult to contain and
the safety of personnel taking the sample is endangered, particularly where pulp
is hot and/or contains hazardous chemicals.
In practice, the valve will probably only be opened partially, which has a signifi-
cant effect on the accuracy and repeatability of the sample.
Consider the following recommendations if you still choose to use a common ball
valve as a sampling valve:
• Select a valve that is large enough, typically over 1”, preferably a 11/2“con-
nection. It ought to be possible to open the valve fully to allow an even,
homogenous flow without overfilling the sampling vessel too quickly.
• Preferably use this method only with low consistencies and short fibers at
under 3% consistency. Avoid it with long-fibered pulps with more than 2%
consistency.
• Ensure that the valve is always fully opened, irrespective of who is using it.
Train your personnel in the procedures.
• Do not use this method with hot pulp of > ≈ 50°C, particularly when there are
hazardous or corrosive chemicals. Avoid the method at pipe pressures
greater than approx. 3 bar.
• Ensure that the sampling personnel wear protective clothing as well as pro-
tective guards and gloves that completely cover the face and hands.
185
Specially-designed sampling valves
Two main types of valve are available for normal consistencies (≤ approx. 8%):
plunger valves and sluice valves with plungers.
Plunger valves
Plunger valves have been on the market for a long time and are manufactured by
several suppliers. The original model has a large opening area and takes its sam-
ple right by the pipe wall (see Fig. 8.2). A cone is pressed into the pulp flow using
a lever so that the pulp pours out. The pulp pours out while the cone is pressed
in. When the lever is released, the valve closes with the help of a spring and the
available pipe pressure. This type of valve gives a sample as doubtful as the ball
valve’s. Its only advantage is that it does not clog as easily (which is another great
drawback of the ball valve).
Fig. 8.2 Sampling valve for pulp, plunger valve, Karl Widenmann
Another type of plunger valve available on the market is one where a cylindrical
plunger is drawn back using a crank so that the pulp is released forwards. As
with the valves previously mentioned, the sample is taken by the pipe wall and
there is a great risk of the valve opening only partially so that de-watering can oc-
cur.
The original plunger valve was further developed during the mid-1980s so that
the sample is now taken far into the pipe where it is more representative. The
flow can be limited and the sample extracted in a more controlled way by limiting
the opening area. Pulp velocity becomes very fast at the opening point and can
also be fluidized. This means that the problem of de-watering is reduced and the
sample will be more representative. One problem with this type of valve is that
the valve opening is not defined; different people can open the valve by differing
amounts and encounter de-watering at low percentage openings.
This type of valve was further developed during the mid-1990s. Its repeatability
is increased by ensuring that the valve always opens to the same percentage. This
is done by the cone being shot out by spring force to full valve opening when the
lever is pushed in (see Fig. 8.3).
186
Water flushing
Fig. 8.3 Sampling valve for pulp, improved plunger valve, BTG type MPS-1000
Fig. 8.4 Sampling valve for pulp, sluice valve with pistons. BTG type VXK-10
187
Sampling higher consistencies and contaminated
pulp
The normal sampling valves described above are not suitable for consistencies
above approx. 8%, and where residual knots or large amounts of shives occur. At
present, there is no really representative sampling device on the market.
One way in which the ball valve can be used in higher consistencies is to construct
a device as illustrated in Fig. 8.5. Here, you have a ball valve with a large flow
(valve A) right next to the pipeline. A flush valve (not shown in Fig 8.5) can be
connected before the pulp valve, to combat plugging. Another flush valve (B) is
used to flush the equipment clean when sampling has been completed. The pulp
flow is diverted in a cyclone so that it can be handled in a controlled manner.
Thanks to the cyclone, the pulp valve (valve A) can be fully opened.
Sample
bucket
Fig. 8.5 Sampling arrangement with ball valves and cyclone for MC
188
Flushing water
Plunger
Fig. 8.6 Sampling valve with plunger for MC. Type Nove H, Valmet Automation
189
Variable-speed controlled pumps constitute another factor that is difficult to as-
sess, as the pulp can be very poorly mixed after these. If possible, a special pulp
mixer should be used in such cases (for consistency control) and in other cases,
the distance is increased to a maximum from the pump to the measurement/sam-
pling point. See Chapter 2.
190
Verifying samples previously taken
If, during regular monitoring, a deviation is noticed, a new sample should be ex-
tracted using the same accuracy requirement as for calibration. No adjustment
should be made to the transmitter until it is established whether deviation origi-
nated in the transmitter or the monitoring sample.
Suitable procedures and documentation should be agreed upon and established
to guarantee and verify accurate sample handling and analysis. Personnel must
implement them faithfully.
Examples of details included in these procedures are as follows:
• Each process department establishes a unique ‘frequency schedule’ for the
various sampling positions.
• The frequency table specifies how often and for which process conditions
consistency samples must be extracted, based on how important the meas-
urement position is.
• There must also be a standard procedure for each sample position, specifying
location, protection/safety, equipment, implementation of sampling, process-
ing the sample, the implementation of the analysis, reporting and what to do
if a value shows deviation.
It is advantageous for the procedures to be included in the documentation for ISO
9000 certification. Drawing up this documentation establishes clear objectives, as
well as limitations and ambitions for all those involved. It enables procedures to
be accurately carried out, which can be measured and evaluated in future, result-
ing in improvements.
191
The following points deserve consideration:
• Representative consistency. Is the sample taken in a position that is repre-
sentative (i.e. are the conditions correct in the pipe from which the sample is
being taken)? Is the pulp of the same composition as during calibration of the
transmitter or at the time of taking the previous sample?
Are samples taken at different consistencies, different flows or different pipe
pressures in the same position? Does the sampling valve function in the same
way when these different conditions occur?
• Correlation with the measurement transmitter. Certain measurement trans-
mitters collate their measurement values over a given time period (e.g. 30
seconds) and present a mean value during this period, to avoid the effect of
rapid consistency oscillations.
How should the sample be extracted to tally with the transmitter’s collated
measurement data? Should a large sample volume be taken and then divided
into sub-samples to form a mean value, or should several individual, sub-
samples be taken during this period? The answer depends on how rapidly
the consistency actually changes. An investigation, whereby many sub-sam-
ples are taken during one period, may provide the answer.
• Variation between different laboratory personnel. Statistically speaking,
there is a difference of approx. ±5-6% in the measurement results of two labo-
ratory technicians who process and analyze one and the same sample.
• Accuracy of individual tests. One investigation at an American mill estab-
lished the following: ‘Under optimal laboratory conditions, a single consist-
ency test produces an error of ±14.1% (within a 95% confidence interval)’. In
other words, a single test value at 2.5% consistency tells us that the actual
consistency lies somewhere between 2.1% and 2.8%. Naturally, this may vary
depending on the circumstances, but it still gives an indication of actual con-
ditions.
• The number of sub-samples and their uncertainty. Three or five sub-sam-
ples are taken from a large sample for analysis, in order to increase the relia-
bility of that analysis. It is then important for the sample to be mixed well and
for the sub-sample to be taken in a uniform way each time. If you have a
beaker, the sample should be taken so that it fills the beaker immediately
with no de-watering at the beaker's lip. At consistencies higher than 3%, it is
often beneficial if the main sample is first diluted with a well-defined quan-
tity of water and then agitated well. In this case, you must know exactly how
much it has been diluted, in order to compensate later.
Suppose that sub-samples show the following values:
Sample 1: 3.02%
Sample 2: 3.00%
Sample 3: 3.10%
192
The average value = 3.04% consistency, with statistically established uncer-
tainty in laboratory sampling, can be a minimum of 2.94% and a maximum of
3.14%. Using probability tables, it is possible to determine that error probabil-
ity for different numbers of sub-samples is as follows:
3 sub-samples: The probability of the mean value being the actual result is
8%, and 50% of the real value being within the range of ±0.04% variation
from the mean value.
5 sub-samples: The probability of the mean value being the actual result is
10%, and 50% of the real value being within the range of ±0.03% variation
from the mean value.
Dividing sampling into 5 sub-samples therefore gives a considerably greater
probability that the sample will tally with the actual result. If one individual
sample deviates substantially from the others, this is rejected since it is proba-
bly erroneous. Please see The Consistency Control Book from Tappi for fur-
ther information in this issue.
Practical recommendations to establish the repeatability of sampling
One suggestion for determining the uncertainty of sampling is to follow the ex-
ample set by one of the Swedish pulp mills we visited in preparation for this
handbook. They began the investigation by carrying out an evaluation test. This
test involved taking samples at equal intervals at a specific consistency level (e.g.
3%) at a measurement position. A particular laboratory technician then extracted
around 20 sub-samples for analysis. It was then possible to draw conclusions
from this investigation regarding the accuracy of sampling. The following level
of accuracy was found at this mill:
• Repeatability during the analysis at the bleaching plant (where conditions are
good) was calculated to be between ±2-3% of the average consistency value.
• In the screening plant (where shives and knots commonly occur), it is more
difficult to analyze the sample to a high level of accuracy; the repeatability
was found to be ±5–6% of the average consistency level.
N.B.: As established earlier, the consistency transmitter usually provides a sub-
stantially greater degree of accuracy than the laboratory samples taken, provided
that a suitable transmitter is selected, correctly located and installed, and proper-
ly maintained. If deviations are established between the transmitter and the lab-
oratory value, it is usually worthwhile to first search for the error in the
laboratory test. However, if a deviation suddenly occurs and remains, the trans-
mitter should also be examined.
193
Accurate analysis of consistency samples
Standards have been established for analysis procedures, in order to ensure the
best level of accuracy. Commonly used standards include the US TAPPI standard
T 240 om-88 to determine consistency, and TAPPI T 211 om-88 to determine ash
content. Corresponding European standards are SCAN-M1:64 to determine con-
sistency and SCAN-C6:62 to determine ash content.
In practice, however, these standards are rarely applied in their entirety, because
of their complexity. Instead, laboratories at individual mills have drawn up their
own simplified procedures, based on one or more of these standards as well as
the mill’s current accuracy requirements and available resources.
The procedure detailed below was obtained from a high-standard Swedish pulp
mill, for use in its bleaching plant, where samples are taken at the normal consist-
ency of 3-4%. It is so general that it is applicable in most cases.
Conditions for MC are different, and also vary from case to case. Binding between
fibers can vary considerably, which affects the accuracy of the sample treatment.
Generally speaking, the sample is treated in a way that avoids de-watering. This
is very important, and great care must be taken.
At the digester, washing and screening plants, requirements are often less strin-
gent than these instructions specify. The closer one comes to the paper machine,
however, the more stringent the control must become.
Analysis equipment
Scales for weighing wet and dry pulp samples to a level of 0.01 grams accuracy.
Sheet mould with wire bottom or Büchner funnel with paper filter. A wire cloth
or paper filter can be used, depending on the level of accuracy desired. With
pulps that are easy to drain, the opening can be 5 µm. With pulps that are difficult
to de-water and which contain filler or fines (fine fractionation), use openings as
small as 3 µm in order to collect as much as possible. If filter paper is used, it
should be dried and stored in a de-moisturizing vessel. The filter paper should be
weighed before being used, and its weight subtracted from the pulp sample.
Water-driven vacuum suction or pump to draw water away from the fiber cake.
Hand mixer to mix the pulp.
194
Ventilated drying cabinet approx. 105 °C – 150 °C. Typically, the temperature
should be 105°C; excessive temperatures may burn the sample and cause incor-
rect weight reduction.
195
Note: if the 3 sub-samples vary considerably, the repeatability of the sampling
procedure must be established. See page 188, and the corrective actions to be tak-
en.
If, occasionally, one sample deviates dramatically from the majority, it should be
deleted when calculating the mean value.
196
Monitoring
Documentation and monitoring of samples (and their relation to the transmitter’s
reading) should be kept in some form. Following is an example of a Swedish
mill’s method.
When the analysis has been carried out, the result is entered in a journal. In this
case, the result is also documented to one decimal point in a computer-based lab-
oratory monitoring program, where users have access to laboratory data from the
process via the internal computer network.
In this particular case, a special computer-controlled analysis device is used to
compare laboratory values and measurement values. Trends and deviations can
be seen, and you gain an idea of the accuracy of the laboratory values and the
measurement transmitter (see Fig. 8.8).
MoDo
V-INFO
97-10-15
07:53:12
No. of Average Deviation Minimum Maximum
samplings
A - Entrance, bleach plant 4, lab. val. % 13 3.554 0.097 3.400 3.700
B - Entrance, bleach plant 4, meas. val. % 13 3.446 0.105 3.300 3.700
C - Entrance, screening plant 4, lab. val. % 18 2.878 0.180 2.400 3.100
D - Entrance, screening plant 4, meas. val. % 18 2.728 0.235 2.200 3.100
5.000
B
A
2.500 C
D
0.000
15/09 22/09 29/09 06/10
197
Smart data collectors are also available. These are connected to the consistency
transmitter (Fig. 8.9). When the sample is taken from the pipe, the current calcu-
lated consistency value from the transmitter is read simultaneously and stored
automatically. Input values can then easily be transferred to a PC, where the lab-
oratory value will be entered later. Regression and correlation between the trans-
mitter and the laboratory can then be seen in a special monitoring program and
can be easily monitored over time (see Fig. 8.10). This is a simple system which
also suits smaller mills. It is adapted to the Swedish SSG standard.
Fig. 8.9 Smart data collector for transmitter data, type SLS-1000, BTG
198
Corrective action
In the current example, this equipment is used to transfer the measurement value
from the transmitter to the analysis computer.
If a deviation exceeding ±0.3% consistency is detected between laboratory and
measured value, an offset adjustment to the transmitter is usually initiated, based
on a verified laboratory test.
In the event of more substantial deviations, or after the transmitter has been re-
paired, 3-point calibration is carried out, based on three different consistency lev-
els such as 2.5, 3.0 and 3.5% pulp consistency.
199
200